Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'R Puddephatt' _publ_contact_author_address ; Department of Chemistry The University of Western Ontario London Ontario N6A 5B7 CANADA ; _publ_contact_author_email PUDD@UWO.CA _publ_section_title ; Ring-Opening Polymerization of Coordination Complexes: Silver(I) Complexes with Bis(Amidopyridine) Ligands Derived from Thiophene ; loop_ _publ_author_name R.Puddephatt 'Michael C. Jennings' 'Nancy Yue' # Attachment 'newcifs.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 604509' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cl2 N4 O6 S' _chemical_formula_weight 497.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.3269(2) _cell_length_b 14.7324(5) _cell_length_c 19.1904(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2354.19(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3065 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description shoebox _exptl_crystal_colour colourless _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7169 _exptl_absorpt_correction_T_max 0.9234 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24629 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2162 _reflns_number_gt 1628 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1722P)^2^+6.2599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2162 _refine_ls_number_parameters 165 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.2833 _refine_ls_wR_factor_gt 0.2588 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 N11 N -0.5839(5) 0.5582(4) -0.0722(3) 0.0437(14) Uani 1 1 d . . . H11A H -0.6796 0.5693 -0.0547 0.052 Uiso 1 1 calc R . . C12 C -0.4597(7) 0.6112(4) -0.0539(3) 0.0374(14) Uani 1 1 d . . . H12A H -0.4762 0.6593 -0.0217 0.045 Uiso 1 1 calc R . . C13 C -0.3098(6) 0.5972(3) -0.0810(3) 0.0307(12) Uani 1 1 d . . . H13A H -0.2222 0.6345 -0.0673 0.037 Uiso 1 1 calc R . . C14 C -0.2874(6) 0.5268(3) -0.1292(3) 0.0269(11) Uani 1 1 d . . . C15 C -0.4193(6) 0.4711(4) -0.1447(3) 0.0352(13) Uani 1 1 d . . . H15A H -0.4065 0.4207 -0.1752 0.042 Uiso 1 1 calc R . . C16 C -0.5650(7) 0.4890(4) -0.1162(3) 0.0424(15) Uani 1 1 d . . . H16A H -0.6544 0.4519 -0.1277 0.051 Uiso 1 1 calc R . . N17 N -0.1376(5) 0.5070(3) -0.1591(2) 0.0255(10) Uani 1 1 d . . . C18 C -0.1035(7) 0.4124(3) -0.1774(3) 0.0363(13) Uani 1 1 d . . . H18A H -0.1488 0.3990 -0.2234 0.054 Uiso 1 1 calc R . . H18B H -0.1519 0.3721 -0.1426 0.054 Uiso 1 1 calc R . . H18C H 0.0129 0.4028 -0.1784 0.054 Uiso 1 1 calc R . . C19 C -0.0180(6) 0.5698(3) -0.1710(2) 0.0225(11) Uani 1 1 d . . . O20 O 0.1200(4) 0.5464(2) -0.18366(18) 0.0287(9) Uani 1 1 d . . . C21 C -0.0642(5) 0.6676(3) -0.1771(2) 0.0225(11) Uani 1 1 d . . . C22 C -0.1864(6) 0.7025(3) -0.2158(2) 0.0278(11) Uani 1 1 d . . . H22A H -0.2629 0.6665 -0.2401 0.042 Uiso 1 1 calc R . . S23 S 0.05417(19) 0.7500 -0.14088(9) 0.0226(6) Uani 1 2 d S . . Cl24 Cl -0.9020(2) 0.58934(14) -0.00745(11) 0.0691(7) Uani 1 1 d . . . O3 O 0.4178(6) 0.7500 0.1972(3) 0.0359(13) Uani 1 2 d SD . . H3A H 0.512(4) 0.7500 0.185(5) 0.054 Uiso 1 2 d SD . . H3B H 0.349(8) 0.7500 0.228(3) 0.054 Uiso 1 2 d SD . . O4 O 0.3463(8) 0.7500 0.0451(3) 0.0488(15) Uani 1 2 d SD . . H4A H 0.387(9) 0.7500 0.085(2) 0.073 Uiso 1 2 d SD . . H4B H 0.249(3) 0.7500 0.054(4) 0.073 Uiso 1 2 d SD . . O5 O -0.0880(9) 0.7500 0.0309(4) 0.067(2) Uani 1 2 d SD . . H5A H -0.181(13) 0.7500 0.047(14) 0.101 Uiso 0.50 2 d SPD A 1 H5B H -0.10(4) 0.7500 -0.012(3) 0.101 Uiso 0.50 2 d SPD B 1 H5C H -0.07(3) 0.798(8) 0.008(9) 0.101 Uiso 0.50 1 d PD C 2 O6 O -0.2447(6) 0.7500 0.1669(3) 0.0262(11) Uiso 1 2 d SD . . H6A H -0.245(7) 0.8029(14) 0.170(3) 0.039 Uiso 1 1 d 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 N11 0.020(2) 0.054(3) 0.056(3) 0.028(3) 0.008(2) 0.008(2) C12 0.039(3) 0.035(3) 0.038(3) 0.011(2) 0.007(2) 0.009(3) C13 0.025(3) 0.032(3) 0.036(3) 0.005(2) 0.004(2) 0.001(2) C14 0.022(2) 0.028(3) 0.030(3) 0.010(2) -0.0017(19) 0.001(2) C15 0.028(3) 0.034(3) 0.043(3) 0.011(2) -0.007(2) -0.005(2) C16 0.028(3) 0.042(3) 0.057(4) 0.016(3) -0.005(3) -0.004(3) N17 0.024(2) 0.021(2) 0.032(2) 0.0031(17) -0.0003(17) 0.0004(17) C18 0.036(3) 0.022(3) 0.051(3) -0.003(2) 0.007(2) -0.002(2) C19 0.023(2) 0.023(2) 0.021(2) 0.0010(19) -0.0033(18) -0.002(2) O20 0.0199(17) 0.0271(19) 0.039(2) 0.0039(15) 0.0028(14) 0.0025(14) C21 0.021(2) 0.021(2) 0.025(2) 0.0012(19) 0.0008(18) -0.0009(19) C22 0.029(3) 0.026(2) 0.028(2) 0.000(2) -0.006(2) -0.001(2) S23 0.0180(9) 0.0221(9) 0.0276(10) 0.000 -0.0029(6) 0.000 Cl24 0.0608(13) 0.0664(13) 0.0803(14) 0.0111(10) -0.0029(9) -0.0018(9) O3 0.034(3) 0.028(3) 0.046(3) 0.000 0.011(3) 0.000 O4 0.065(4) 0.043(3) 0.038(3) 0.000 0.003(3) 0.000 O5 0.049(4) 0.112(7) 0.042(4) 0.000 0.005(3) 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 N11 C16 1.334(8) . ? N11 C12 1.342(8) . ? C12 C13 1.368(7) . ? C13 C14 1.403(7) . ? C14 N17 1.403(6) . ? C14 C15 1.403(7) . ? C15 C16 1.357(8) . ? N17 C19 1.379(6) . ? N17 C18 1.465(6) . ? C19 O20 1.224(6) . ? C19 C21 1.496(7) . ? C21 C22 1.361(7) . ? C21 S23 1.711(5) . ? C22 C22 1.400(10) 7_575 ? S23 C21 1.711(5) 7_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 N11 C12 121.3(5) . . ? N11 C12 C13 121.1(6) . . ? C12 C13 C14 118.9(5) . . ? N17 C14 C13 122.7(4) . . ? N17 C14 C15 119.2(5) . . ? C13 C14 C15 118.0(5) . . ? C16 C15 C14 120.0(6) . . ? N11 C16 C15 120.7(5) . . ? C19 N17 C14 124.7(4) . . ? C19 N17 C18 117.3(4) . . ? C14 N17 C18 117.9(4) . . ? O20 C19 N17 121.4(4) . . ? O20 C19 C21 119.8(4) . . ? N17 C19 C21 118.3(4) . . ? C22 C21 C19 126.8(4) . . ? C22 C21 S23 112.6(4) . . ? C19 C21 S23 120.2(3) . . ? C21 C22 C22 112.2(3) . 7_575 ? C21 S23 C21 90.3(3) . 7_575 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11A Cl24 0.88 2.08 2.961(5) 175.9 . O3 H3A O6 0.82(2) 2.06(2) 2.869(7) 173(10) 1_655 O3 H3B O6 0.83(2) 2.15(4) 2.939(7) 158(9) 6_656 O4 H4A O3 0.84(2) 2.17(4) 2.979(8) 163(8) . O5 H5A O6 0.83(2) 2.4(2) 2.918(9) 124(24) . O5 H5B S23 0.84(2) 2.8(2) 3.503(7) 144(28) . O5 H5C Cl24 0.83(2) 2.22(12) 2.923(5) 143(18) 7_675 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.688 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.138 #===END data_8a _database_code_depnum_ccdc_archive 'CCDC 604510' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H34 Ag2 Cl2 F6 N8 O8 S2' _chemical_formula_weight 1231.52 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' 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 11.6130(5) _cell_length_b 14.0366(5) _cell_length_c 16.2974(6) _cell_angle_alpha 65.287(2) _cell_angle_beta 81.037(2) _cell_angle_gamma 72.264(2) _cell_volume 2297.34(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6647 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6386 _exptl_absorpt_correction_T_max 0.7398 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23618 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.62 _reflns_number_total 10374 _reflns_number_gt 7432 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0415P)^2^+0.7880P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10374 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.00002(2) 1.11715(2) -0.997311(15) 0.03582(9) Uani 1 1 d . . . Ag2 Ag -0.02111(3) 0.61545(2) -1.005294(18) 0.05068(11) Uani 1 1 d . . . N11 N 0.0684(2) 1.1969(2) -1.13522(15) 0.0274(6) Uani 1 1 d . . . C12 C 0.1782(3) 1.2147(3) -1.1547(2) 0.0324(8) Uani 1 1 d . . . H12A H 0.2327 1.1845 -1.1069 0.039 Uiso 1 1 calc R . . C13 C 0.2168(3) 1.2742(3) -1.2402(2) 0.0305(7) Uani 1 1 d . . . H13A H 0.2961 1.2837 -1.2504 0.037 Uiso 1 1 calc R . . C14 C 0.1389(3) 1.3199(2) -1.31091(19) 0.0236(7) Uani 1 1 d . . . C15 C 0.0241(3) 1.3028(2) -1.29192(19) 0.0237(6) Uani 1 1 d . . . H15A H -0.0328 1.3338 -1.3383 0.028 Uiso 1 1 calc R . . C16 C -0.0058(3) 1.2401(2) -1.20468(19) 0.0260(7) Uani 1 1 d . . . H16A H -0.0834 1.2268 -1.1931 0.031 Uiso 1 1 calc R . . N17 N 0.1738(2) 1.38799(19) -1.39846(16) 0.0254(6) Uani 1 1 d . . . C18 C 0.2459(3) 1.4615(3) -1.4039(2) 0.0330(8) Uani 1 1 d . . . H18A H 0.2638 1.5035 -1.4675 0.050 Uiso 1 1 calc R . . H18B H 0.3218 1.4182 -1.3727 0.050 Uiso 1 1 calc R . . H18C H 0.1998 1.5113 -1.3753 0.050 Uiso 1 1 calc R . . C19 C 0.1331(2) 1.4007(2) -1.47885(19) 0.0238(7) Uani 1 1 d . . . O20 O 0.13550(19) 1.48201(16) -1.54709(13) 0.0291(5) Uani 1 1 d . . . N21 N -0.1782(2) 0.7124(2) -1.08460(18) 0.0354(7) Uani 1 1 d . . . C22 C -0.1704(3) 0.7712(3) -1.1734(2) 0.0322(8) Uani 1 1 d . . . H22A H -0.0929 0.7647 -1.2030 0.039 Uiso 1 1 calc R . . C23 C -0.2697(3) 0.8406(2) -1.2236(2) 0.0270(7) Uani 1 1 d . . . H23A H -0.2609 0.8823 -1.2864 0.032 Uiso 1 1 calc R . . C24 C -0.3827(3) 0.8485(2) -1.18085(19) 0.0234(6) Uani 1 1 d . . . C25 C -0.3918(3) 0.7880(2) -1.0887(2) 0.0288(7) Uani 1 1 d . . . H25A H -0.4681 0.7924 -1.0573 0.035 Uiso 1 1 calc R . . C26 C -0.2879(3) 0.7218(3) -1.0444(2) 0.0359(8) Uani 1 1 d . . . H26A H -0.2942 0.6801 -0.9814 0.043 Uiso 1 1 calc R . . N27 N -0.4875(2) 0.91968(19) -1.22904(16) 0.0234(5) Uani 1 1 d . . . C28 C -0.5669(3) 0.9994(2) -1.1949(2) 0.0309(7) Uani 1 1 d . . . H28A H -0.6355 1.0430 -1.2347 0.046 Uiso 1 1 calc R . . H28B H -0.5215 1.0472 -1.1935 0.046 Uiso 1 1 calc R . . H28C H -0.5968 0.9614 -1.1337 0.046 Uiso 1 1 calc R . . C29 C -0.5058(3) 0.9316(2) -1.31431(19) 0.0237(7) Uani 1 1 d . . . O30 O -0.57351(19) 1.01401(16) -1.36524(13) 0.0335(5) Uani 1 1 d . . . N31 N 0.0579(2) 0.9143(2) -1.14345(15) 0.0284(6) Uani 1 1 d . . . C32 C 0.1697(3) 0.8637(2) -1.1630(2) 0.0297(7) Uani 1 1 d . . . H32A H 0.2245 0.8209 -1.1152 0.036 Uiso 1 1 calc R . . C33 C 0.2091(3) 0.8703(2) -1.24808(19) 0.0269(7) Uani 1 1 d . . . H33A H 0.2891 0.8320 -1.2582 0.032 Uiso 1 1 calc R . . C34 C 0.1325(3) 0.9327(2) -1.31974(19) 0.0213(6) Uani 1 1 d . . . C35 C 0.0166(3) 0.9858(2) -1.30049(19) 0.0229(6) Uani 1 1 d . . . H35A H -0.0395 1.0293 -1.3473 0.028 Uiso 1 1 calc R . . C36 C -0.0165(3) 0.9749(2) -1.21265(19) 0.0265(7) Uani 1 1 d . . . H36A H -0.0961 1.0123 -1.2006 0.032 Uiso 1 1 calc R . . N37 N 0.1702(2) 0.93546(18) -1.40717(15) 0.0227(5) Uani 1 1 d . . . C38 C 0.2415(3) 0.8327(2) -1.4140(2) 0.0331(8) Uani 1 1 d . . . H38A H 0.2621 0.8451 -1.4776 0.050 Uiso 1 1 calc R . . H38B H 0.1941 0.7792 -1.3882 0.050 Uiso 1 1 calc R . . H38C H 0.3160 0.8052 -1.3806 0.050 Uiso 1 1 calc R . . C39 C 0.1392(3) 1.0235(2) -1.48732(19) 0.0260(7) Uani 1 1 d . . . O40 O 0.1489(2) 1.01215(18) -1.55851(14) 0.0363(6) Uani 1 1 d . . . N41 N -0.1241(2) 0.4421(2) -1.08620(17) 0.0343(7) Uani 1 1 d . . . C42 C -0.1101(3) 0.4895(3) -1.1764(2) 0.0330(8) Uani 1 1 d . . . H42A H -0.0404 0.5155 -1.2006 0.040 Uiso 1 1 calc R . . C43 C -0.1913(3) 0.5021(2) -1.2353(2) 0.0284(7) Uani 1 1 d . . . H43A H -0.1779 0.5358 -1.2988 0.034 Uiso 1 1 calc R . . C44 C -0.2937(3) 0.4647(2) -1.20060(19) 0.0230(6) Uani 1 1 d . . . C45 C -0.3116(3) 0.4195(3) -1.1076(2) 0.0334(8) Uani 1 1 d . . . H45A H -0.3821 0.3955 -1.0816 0.040 Uiso 1 1 calc R . . C46 C -0.2254(3) 0.4102(3) -1.0542(2) 0.0373(8) Uani 1 1 d . . . H46A H -0.2383 0.3793 -0.9905 0.045 Uiso 1 1 calc R . . N47 N -0.3756(2) 0.46665(19) -1.25802(16) 0.0249(6) Uani 1 1 d . . . C48 C -0.3982(3) 0.3620(2) -1.2396(2) 0.0344(8) Uani 1 1 d . . . H48A H -0.4555 0.3726 -1.2829 0.052 Uiso 1 1 calc R . . H48B H -0.4322 0.3333 -1.1781 0.052 Uiso 1 1 calc R . . H48C H -0.3220 0.3104 -1.2457 0.052 Uiso 1 1 calc R . . C49 C -0.4060(3) 0.5498(2) -1.34076(19) 0.0247(7) Uani 1 1 d . . . O50 O -0.43887(19) 0.53473(17) -1.40115(14) 0.0308(5) Uani 1 1 d . . . C51 C 0.1049(3) 1.1359(2) -1.49035(18) 0.0235(6) Uani 1 1 d . . . C52 C 0.0451(3) 1.2238(2) -1.56080(19) 0.0269(7) Uani 1 1 d . . . H52A H 0.0091 1.2185 -1.6067 0.032 Uiso 1 1 calc R . . C53 C 0.0428(3) 1.3222(2) -1.55784(19) 0.0258(7) Uani 1 1 d . . . H53A H 0.0046 1.3911 -1.6018 0.031 Uiso 1 1 calc R . . C54 C 0.1006(2) 1.3102(2) -1.48559(18) 0.0216(6) Uani 1 1 d . . . S55 S 0.15801(7) 1.17471(6) -1.41969(5) 0.02319(17) Uani 1 1 d . . . C61 C -0.4532(2) 0.8383(2) -1.34030(18) 0.0220(6) Uani 1 1 d . . . C62 C -0.4236(3) 0.8443(2) -1.42663(19) 0.0259(7) Uani 1 1 d . . . H62A H -0.4195 0.9097 -1.4769 0.031 Uiso 1 1 calc R . . C63 C -0.3999(3) 0.7432(2) -1.43271(19) 0.0249(7) Uani 1 1 d . . . H63A H -0.3785 0.7331 -1.4878 0.030 Uiso 1 1 calc R . . C64 C -0.4106(2) 0.6614(2) -1.35192(19) 0.0227(6) Uani 1 1 d . . . S65 S -0.44957(7) 0.70700(6) -1.26607(5) 0.02332(17) Uani 1 1 d . . . O71 O 0.1309(2) 0.5378(3) -1.10307(17) 0.0705(10) Uani 1 1 d . . . O72 O 0.1024(2) 0.6398(3) -1.25062(18) 0.0678(10) Uani 1 1 d . . . C73 C 0.1618(3) 0.5768(3) -1.1841(2) 0.0408(9) Uani 1 1 d . . . C74 C 0.2958(3) 0.5349(3) -1.2008(2) 0.0377(8) Uani 1 1 d . . . F75 F 0.3245(2) 0.42737(18) -1.18141(16) 0.0775(9) Uani 1 1 d . . . F76 F 0.3642(2) 0.5458(2) -1.14984(16) 0.0736(8) Uani 1 1 d . . . F77 F 0.33540(17) 0.57847(16) -1.28589(13) 0.0470(6) Uani 1 1 d . . . O81 O -0.1570(2) 1.07803(18) -1.06056(15) 0.0383(6) Uani 1 1 d . . . O82 O -0.3185(2) 1.17328(18) -1.00562(15) 0.0360(6) Uani 1 1 d . . . C83 C -0.2675(3) 1.1134(2) -1.04476(19) 0.0282(7) Uani 1 1 d . . . C84 C -0.3488(3) 1.0737(3) -1.0821(2) 0.0312(7) Uani 1 1 d . . . F85 F -0.3429(3) 0.96993(18) -1.03427(17) 0.0750(8) Uani 1 1 d . . . F86 F -0.31955(19) 1.08508(19) -1.16775(13) 0.0536(6) Uani 1 1 d . . . F87 F -0.46500(18) 1.1270(2) -1.08359(16) 0.0586(6) Uani 1 1 d . . . C90 C -0.3661(3) 1.3108(2) -1.4388(2) 0.0331(8) Uani 1 1 d . . . H90A H -0.3688 1.3257 -1.5036 0.040 Uiso 1 1 calc R . . H90B H -0.4006 1.3805 -1.4312 0.040 Uiso 1 1 calc R . . Cl91 Cl -0.45409(9) 1.21964(8) -1.37421(6) 0.0474(2) Uani 1 1 d . . . Cl92 Cl -0.21466(8) 1.25620(7) -1.40506(6) 0.0430(2) 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 0.04509(17) 0.04114(16) 0.01490(12) -0.00590(11) 0.00349(11) -0.01243(12) Ag2 0.03913(17) 0.0615(2) 0.03772(17) -0.01125(15) -0.02219(13) 0.00373(14) N11 0.0346(15) 0.0285(14) 0.0142(12) -0.0052(11) 0.0052(11) -0.0092(11) C12 0.0386(19) 0.0372(18) 0.0194(16) -0.0067(14) -0.0041(14) -0.0123(15) C13 0.0293(17) 0.0363(18) 0.0243(16) -0.0065(14) -0.0020(13) -0.0137(14) C14 0.0290(16) 0.0187(14) 0.0207(15) -0.0075(12) 0.0029(12) -0.0053(12) C15 0.0246(15) 0.0246(15) 0.0182(14) -0.0070(12) -0.0014(12) -0.0034(12) C16 0.0272(16) 0.0274(16) 0.0202(15) -0.0081(13) 0.0015(12) -0.0059(13) N17 0.0297(14) 0.0258(13) 0.0187(12) -0.0046(11) 0.0018(10) -0.0118(11) C18 0.0384(19) 0.0316(18) 0.0283(17) -0.0061(14) 0.0010(14) -0.0175(15) C19 0.0197(14) 0.0231(15) 0.0193(15) -0.0046(13) 0.0046(12) -0.0012(12) O20 0.0367(12) 0.0219(11) 0.0198(11) -0.0004(9) 0.0004(9) -0.0074(9) N21 0.0305(15) 0.0401(16) 0.0289(15) -0.0097(13) -0.0146(12) 0.0010(12) C22 0.0243(16) 0.0388(19) 0.0329(18) -0.0130(15) -0.0078(14) -0.0057(14) C23 0.0250(16) 0.0304(17) 0.0219(15) -0.0061(13) -0.0066(12) -0.0056(13) C24 0.0262(16) 0.0208(15) 0.0239(15) -0.0091(12) -0.0056(12) -0.0047(12) C25 0.0315(17) 0.0301(17) 0.0213(16) -0.0083(13) -0.0018(13) -0.0054(13) C26 0.042(2) 0.0375(19) 0.0211(16) -0.0049(14) -0.0081(15) -0.0068(15) N27 0.0236(13) 0.0240(13) 0.0207(12) -0.0099(10) -0.0045(10) -0.0004(10) C28 0.0322(17) 0.0269(17) 0.0302(17) -0.0121(14) -0.0037(14) -0.0006(13) C29 0.0225(15) 0.0225(15) 0.0198(15) -0.0044(12) -0.0004(12) -0.0033(12) O30 0.0379(13) 0.0238(11) 0.0235(11) -0.0018(9) -0.0081(10) 0.0054(10) N31 0.0347(15) 0.0333(14) 0.0134(12) -0.0048(11) 0.0028(11) -0.0119(12) C32 0.0285(17) 0.0320(17) 0.0233(16) -0.0055(14) -0.0077(13) -0.0053(13) C33 0.0243(16) 0.0301(17) 0.0232(16) -0.0095(13) -0.0003(12) -0.0046(13) C34 0.0248(15) 0.0207(15) 0.0200(14) -0.0089(12) 0.0018(12) -0.0084(12) C35 0.0249(15) 0.0249(15) 0.0186(14) -0.0060(12) -0.0021(12) -0.0092(12) C36 0.0255(16) 0.0317(17) 0.0201(15) -0.0089(13) 0.0012(12) -0.0075(13) N37 0.0263(13) 0.0221(13) 0.0172(12) -0.0091(10) 0.0014(10) -0.0023(10) C38 0.0388(19) 0.0309(17) 0.0299(17) -0.0186(14) 0.0013(14) -0.0014(14) C39 0.0259(16) 0.0330(17) 0.0208(15) -0.0110(14) 0.0001(12) -0.0101(13) O40 0.0526(15) 0.0411(13) 0.0202(11) -0.0175(10) -0.0001(10) -0.0121(11) N41 0.0326(15) 0.0372(16) 0.0275(15) -0.0093(12) -0.0152(12) 0.0002(12) C42 0.0244(16) 0.0413(19) 0.0296(18) -0.0130(15) -0.0055(13) -0.0026(14) C43 0.0258(16) 0.0329(17) 0.0217(15) -0.0088(13) -0.0033(13) -0.0030(13) C44 0.0263(15) 0.0187(14) 0.0211(15) -0.0078(12) -0.0052(12) 0.0002(12) C45 0.0410(19) 0.0341(18) 0.0266(17) -0.0072(14) -0.0031(14) -0.0178(15) C46 0.049(2) 0.0385(19) 0.0218(17) -0.0060(15) -0.0066(15) -0.0146(16) N47 0.0318(14) 0.0231(13) 0.0210(13) -0.0087(11) -0.0048(11) -0.0073(11) C48 0.047(2) 0.0288(17) 0.0333(18) -0.0136(15) -0.0051(15) -0.0147(15) C49 0.0222(15) 0.0289(16) 0.0217(15) -0.0114(13) 0.0010(12) -0.0040(12) O50 0.0361(12) 0.0353(12) 0.0267(12) -0.0190(10) -0.0078(10) -0.0044(10) C51 0.0271(16) 0.0262(16) 0.0158(14) -0.0083(12) 0.0022(12) -0.0064(12) C52 0.0250(16) 0.0358(18) 0.0179(15) -0.0081(13) -0.0020(12) -0.0084(13) C53 0.0220(15) 0.0272(16) 0.0181(15) -0.0017(13) -0.0016(12) -0.0028(12) C54 0.0205(14) 0.0218(15) 0.0174(14) -0.0055(12) 0.0027(11) -0.0035(12) S55 0.0287(4) 0.0205(4) 0.0167(3) -0.0049(3) -0.0048(3) -0.0030(3) C61 0.0200(14) 0.0235(15) 0.0176(14) -0.0038(12) -0.0040(11) -0.0035(12) C62 0.0227(15) 0.0261(16) 0.0203(15) -0.0030(13) -0.0027(12) -0.0029(12) C63 0.0244(15) 0.0309(16) 0.0168(14) -0.0102(13) -0.0014(12) -0.0024(12) C64 0.0207(14) 0.0267(16) 0.0202(15) -0.0098(13) -0.0028(12) -0.0038(12) S65 0.0294(4) 0.0219(4) 0.0161(3) -0.0056(3) -0.0012(3) -0.0056(3) O71 0.0441(16) 0.120(3) 0.0313(15) -0.0186(16) 0.0063(12) -0.0189(16) O72 0.0312(14) 0.097(2) 0.0411(16) 0.0038(16) -0.0063(12) -0.0126(14) C73 0.0287(18) 0.064(2) 0.0288(18) -0.0127(18) 0.0021(15) -0.0209(17) C74 0.0367(19) 0.040(2) 0.0321(19) -0.0084(16) -0.0025(15) -0.0123(16) F75 0.102(2) 0.0387(13) 0.0619(16) -0.0072(12) 0.0262(15) -0.0100(13) F76 0.0428(13) 0.134(2) 0.0594(15) -0.0424(16) -0.0076(11) -0.0353(14) F77 0.0385(11) 0.0519(12) 0.0363(11) -0.0063(10) 0.0096(9) -0.0137(9) O81 0.0302(13) 0.0477(14) 0.0370(13) -0.0161(11) 0.0014(10) -0.0124(11) O82 0.0421(14) 0.0362(13) 0.0323(13) -0.0178(11) -0.0040(11) -0.0066(11) C83 0.0355(18) 0.0262(16) 0.0166(15) -0.0004(13) 0.0005(13) -0.0120(14) C84 0.0356(19) 0.0339(18) 0.0244(16) -0.0123(14) 0.0031(14) -0.0106(15) F85 0.118(2) 0.0413(13) 0.0710(17) 0.0010(12) -0.0376(15) -0.0445(14) F86 0.0476(13) 0.0917(17) 0.0347(11) -0.0361(12) 0.0035(10) -0.0229(12) F87 0.0306(11) 0.0853(16) 0.0839(17) -0.0569(14) 0.0059(11) -0.0181(11) C90 0.0404(19) 0.0277(17) 0.0304(18) -0.0111(14) -0.0004(15) -0.0090(14) Cl91 0.0499(5) 0.0512(6) 0.0414(5) -0.0075(4) -0.0091(4) -0.0257(4) Cl92 0.0351(5) 0.0453(5) 0.0515(5) -0.0244(4) 0.0022(4) -0.0088(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N31 2.182(2) 2_573 ? Ag1 N11 2.195(2) . ? Ag1 O81 2.522(2) . ? Ag1 Ag1 3.3265(6) 2_573 ? Ag2 N21 2.145(2) . ? Ag2 N41 2.160(3) 2_563 ? Ag2 O71 2.500(3) . ? Ag2 Ag2 3.0604(7) 2_563 ? N11 C12 1.337(4) . ? N11 C16 1.343(4) . ? C12 C13 1.379(4) . ? C13 C14 1.382(4) . ? C14 C15 1.391(4) . ? C14 N17 1.424(3) . ? C15 C16 1.379(4) . ? N17 C19 1.385(4) . ? N17 C18 1.484(4) . ? C19 O20 1.220(3) . ? C19 C54 1.479(4) . ? N21 C26 1.334(4) . ? N21 C22 1.337(4) . ? C22 C23 1.376(4) . ? C23 C24 1.382(4) . ? C24 C25 1.388(4) . ? C24 N27 1.413(3) . ? C25 C26 1.367(4) . ? N27 C29 1.371(4) . ? N27 C28 1.464(4) . ? C29 O30 1.221(3) . ? C29 C61 1.471(4) . ? N31 C32 1.339(4) . ? N31 C36 1.340(4) . ? N31 Ag1 2.182(2) 2_573 ? C32 C33 1.364(4) . ? C33 C34 1.384(4) . ? C34 C35 1.385(4) . ? C34 N37 1.412(3) . ? C35 C36 1.379(4) . ? N37 C39 1.375(4) . ? N37 C38 1.468(4) . ? C39 O40 1.220(3) . ? C39 C51 1.485(4) . ? N41 C46 1.338(4) . ? N41 C42 1.344(4) . ? N41 Ag2 2.160(3) 2_563 ? C42 C43 1.372(4) . ? C43 C44 1.390(4) . ? C44 C45 1.386(4) . ? C44 N47 1.421(4) . ? C45 C46 1.370(5) . ? N47 C49 1.374(4) . ? N47 C48 1.469(4) . ? C49 O50 1.224(4) . ? C49 C64 1.485(4) . ? C51 C52 1.366(4) . ? C51 S55 1.719(3) . ? C52 C53 1.394(4) . ? C53 C54 1.371(4) . ? C54 S55 1.720(3) . ? C61 C62 1.369(4) . ? C61 S65 1.722(3) . ? C62 C63 1.403(4) . ? C63 C64 1.356(4) . ? C64 S65 1.717(3) . ? O71 C73 1.241(4) . ? O72 C73 1.222(4) . ? C73 C74 1.511(5) . ? C74 F76 1.316(4) . ? C74 F77 1.331(4) . ? C74 F75 1.348(4) . ? O81 C83 1.255(4) . ? O82 C83 1.222(4) . ? C83 C84 1.534(5) . ? C84 F85 1.319(4) . ? C84 F87 1.327(4) . ? C84 F86 1.338(3) . ? C90 Cl92 1.764(3) . ? C90 Cl91 1.767(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 N31 Ag1 N11 160.40(10) 2_573 . ? N31 Ag1 O81 104.94(9) 2_573 . ? N11 Ag1 O81 89.56(9) . . ? N31 Ag1 Ag1 99.54(7) 2_573 2_573 ? N11 Ag1 Ag1 99.81(7) . 2_573 ? O81 Ag1 Ag1 51.81(5) . 2_573 ? N21 Ag2 N41 163.09(11) . 2_563 ? N21 Ag2 O71 106.56(10) . . ? N41 Ag2 O71 86.40(10) 2_563 . ? N21 Ag2 Ag2 106.12(8) . 2_563 ? N41 Ag2 Ag2 90.02(8) 2_563 2_563 ? O71 Ag2 Ag2 56.48(8) . 2_563 ? C12 N11 C16 116.4(2) . . ? C12 N11 Ag1 123.8(2) . . ? C16 N11 Ag1 119.5(2) . . ? N11 C12 C13 123.8(3) . . ? C12 C13 C14 119.3(3) . . ? C13 C14 C15 117.7(3) . . ? C13 C14 N17 120.3(3) . . ? C15 C14 N17 121.8(3) . . ? C16 C15 C14 119.0(3) . . ? N11 C16 C15 123.7(3) . . ? C19 N17 C14 124.8(3) . . ? C19 N17 C18 117.1(2) . . ? C14 N17 C18 117.6(2) . . ? O20 C19 N17 120.3(3) . . ? O20 C19 C54 119.1(3) . . ? N17 C19 C54 120.2(2) . . ? C26 N21 C22 117.7(3) . . ? C26 N21 Ag2 119.9(2) . . ? C22 N21 Ag2 122.2(2) . . ? N21 C22 C23 122.9(3) . . ? C22 C23 C24 118.6(3) . . ? C23 C24 C25 119.0(3) . . ? C23 C24 N27 120.9(3) . . ? C25 C24 N27 120.0(3) . . ? C26 C25 C24 118.1(3) . . ? N21 C26 C25 123.8(3) . . ? C29 N27 C24 122.6(2) . . ? C29 N27 C28 117.9(2) . . ? C24 N27 C28 118.3(2) . . ? O30 C29 N27 121.2(3) . . ? O30 C29 C61 119.8(3) . . ? N27 C29 C61 118.7(2) . . ? C32 N31 C36 116.7(3) . . ? C32 N31 Ag1 119.7(2) . 2_573 ? C36 N31 Ag1 123.3(2) . 2_573 ? N31 C32 C33 123.4(3) . . ? C32 C33 C34 120.1(3) . . ? C33 C34 C35 117.2(3) . . ? C33 C34 N37 120.5(2) . . ? C35 C34 N37 122.3(3) . . ? C36 C35 C34 119.3(3) . . ? N31 C36 C35 123.4(3) . . ? C39 N37 C34 126.2(2) . . ? C39 N37 C38 116.4(2) . . ? C34 N37 C38 117.2(2) . . ? O40 C39 N37 121.1(3) . . ? O40 C39 C51 118.2(3) . . ? N37 C39 C51 120.3(3) . . ? C46 N41 C42 117.0(3) . . ? C46 N41 Ag2 118.4(2) . 2_563 ? C42 N41 Ag2 123.2(2) . 2_563 ? N41 C42 C43 123.2(3) . . ? C42 C43 C44 118.9(3) . . ? C45 C44 C43 118.5(3) . . ? C45 C44 N47 120.0(3) . . ? C43 C44 N47 121.4(3) . . ? C46 C45 C44 118.4(3) . . ? N41 C46 C45 124.0(3) . . ? C49 N47 C44 123.2(2) . . ? C49 N47 C48 118.0(3) . . ? C44 N47 C48 116.3(2) . . ? O50 C49 N47 121.4(3) . . ? O50 C49 C64 120.4(3) . . ? N47 C49 C64 117.9(3) . . ? C52 C51 C39 122.5(3) . . ? C52 C51 S55 111.6(2) . . ? C39 C51 S55 124.8(2) . . ? C51 C52 C53 112.4(3) . . ? C54 C53 C52 113.7(3) . . ? C53 C54 C19 123.1(3) . . ? C53 C54 S55 110.7(2) . . ? C19 C54 S55 124.7(2) . . ? C51 S55 C54 91.62(14) . . ? C62 C61 C29 125.6(3) . . ? C62 C61 S65 111.2(2) . . ? C29 C61 S65 122.0(2) . . ? C61 C62 C63 112.6(3) . . ? C64 C63 C62 113.1(3) . . ? C63 C64 C49 124.1(3) . . ? C63 C64 S65 111.6(2) . . ? C49 C64 S65 123.7(2) . . ? C64 S65 C61 91.43(14) . . ? C73 O71 Ag2 132.7(3) . . ? O72 C73 O71 131.0(3) . . ? O72 C73 C74 116.5(3) . . ? O71 C73 C74 112.5(3) . . ? F76 C74 F77 107.0(3) . . ? F76 C74 F75 105.5(3) . . ? F77 C74 F75 104.6(3) . . ? F76 C74 C73 113.6(3) . . ? F77 C74 C73 115.2(3) . . ? F75 C74 C73 110.1(3) . . ? C83 O81 Ag1 120.4(2) . . ? O82 C83 O81 130.5(3) . . ? O82 C83 C84 116.5(3) . . ? O81 C83 C84 113.0(3) . . ? F85 C84 F87 106.4(3) . . ? F85 C84 F86 107.0(3) . . ? F87 C84 F86 104.3(3) . . ? F85 C84 C83 111.7(3) . . ? F87 C84 C83 114.2(3) . . ? F86 C84 C83 112.7(3) . . ? Cl92 C90 Cl91 110.95(17) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.577 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.093 #===END data_8b _database_code_depnum_ccdc_archive 'CCDC 604511' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H34 Ag2 Cl2 N10 O10 S2' _chemical_formula_weight 1129.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.6444(14) _cell_length_b 12.9349(17) _cell_length_c 15.5919(16) _cell_angle_alpha 68.512(6) _cell_angle_beta 76.221(7) _cell_angle_gamma 73.795(6) _cell_volume 2074.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6043 _exptl_absorpt_correction_T_max 0.8856 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15552 _diffrn_reflns_av_R_equivalents 0.090 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7138 _reflns_number_gt 4113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0895P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7138 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 0.02490(6) 0.61793(5) 0.48850(4) 0.0402(2) Uani 1 1 d . . . Ag2 Ag -0.02492(6) -0.11251(5) 1.50773(4) 0.0427(2) Uani 1 1 d . . . N1 N 0.1782(6) 0.5603(5) 0.5591(4) 0.0374(16) Uani 1 1 d . . . C2 C 0.1684(7) 0.5176(6) 0.6530(5) 0.0356(18) Uani 1 1 d . . . H2A H 0.0943 0.4975 0.6873 0.043 Uiso 1 1 calc R . . C3 C 0.2595(7) 0.5014(6) 0.7021(5) 0.0375(19) Uani 1 1 d . . . H3A H 0.2473 0.4717 0.7683 0.045 Uiso 1 1 calc R . . C4 C 0.3688(7) 0.5290(6) 0.6539(5) 0.0388(19) Uani 1 1 d . . . C5 C 0.3801(7) 0.5749(6) 0.5557(5) 0.0395(19) Uani 1 1 d . . . H5A H 0.4527 0.5970 0.5199 0.047 Uiso 1 1 calc R . . C6 C 0.2853(7) 0.5870(6) 0.5132(5) 0.039(2) Uani 1 1 d . . . H6A H 0.2953 0.6160 0.4470 0.047 Uiso 1 1 calc R . . N7 N 0.4639(6) 0.5172(5) 0.6995(4) 0.0407(16) Uani 1 1 d . . . C8 C 0.5325(8) 0.6082(7) 0.6663(6) 0.065(3) Uani 1 1 d . . . H8A H 0.5954 0.5880 0.7051 0.098 Uiso 1 1 calc R . . H8B H 0.4775 0.6796 0.6703 0.098 Uiso 1 1 calc R . . H8C H 0.5701 0.6176 0.6013 0.098 Uiso 1 1 calc R . . C9 C 0.4881(8) 0.4334(7) 0.7812(6) 0.045(2) Uani 1 1 d . . . O10 O 0.5423(6) 0.4427(5) 0.8347(4) 0.0659(19) Uani 1 1 d . . . C11 C 0.4601(7) 0.3209(7) 0.8003(5) 0.045(2) Uani 1 1 d . . . S12 S 0.46605(19) 0.26470(17) 0.71382(13) 0.0405(5) Uani 1 1 d . . . C13 C 0.4514(7) 0.1344(6) 0.7943(5) 0.0396(19) Uani 1 1 d . . . C14 C 0.4401(7) 0.1343(7) 0.8839(5) 0.047(2) Uani 1 1 d . . . H14A H 0.4289 0.0710 0.9381 0.057 Uiso 1 1 calc R . . C15 C 0.4472(7) 0.2391(7) 0.8848(5) 0.041(2) Uani 1 1 d . . . H15A H 0.4432 0.2530 0.9412 0.049 Uiso 1 1 calc R . . C16 C 0.4702(8) 0.0296(7) 0.7674(6) 0.048(2) Uani 1 1 d . . . O17 O 0.5338(7) -0.0587(5) 0.8082(5) 0.075(2) Uani 1 1 d . . . N18 N 0.4241(6) 0.0414(5) 0.6901(4) 0.0411(17) Uani 1 1 d . . . C19 C 0.4719(8) -0.0483(7) 0.6454(6) 0.056(2) Uani 1 1 d . . . H19A H 0.5382 -0.1040 0.6763 0.084 Uiso 1 1 calc R . . H19B H 0.5019 -0.0141 0.5794 0.084 Uiso 1 1 calc R . . H19C H 0.4072 -0.0864 0.6510 0.084 Uiso 1 1 calc R . . C20 C 0.3279(7) 0.1295(6) 0.6538(5) 0.0323(18) Uani 1 1 d . . . C21 C 0.2214(7) 0.1607(6) 0.7108(5) 0.0374(19) Uani 1 1 d . . . H21A H 0.2146 0.1280 0.7767 0.045 Uiso 1 1 calc R . . C22 C 0.1276(7) 0.2385(6) 0.6707(5) 0.0367(19) Uani 1 1 d . . . H22A H 0.0550 0.2578 0.7102 0.044 Uiso 1 1 calc R . . N23 N 0.1321(5) 0.2897(5) 0.5781(4) 0.0312(14) Uani 1 1 d . . . C24 C 0.2347(7) 0.2613(7) 0.5238(5) 0.043(2) Uani 1 1 d . . . H24A H 0.2402 0.2969 0.4582 0.052 Uiso 1 1 calc R . . C25 C 0.3336(7) 0.1817(6) 0.5596(5) 0.040(2) Uani 1 1 d . . . H25A H 0.4051 0.1635 0.5188 0.048 Uiso 1 1 calc R . . N31 N -0.0918(6) -0.1986(5) 1.6503(4) 0.0331(15) Uani 1 1 d . . . C32 C -0.0146(7) -0.2648(6) 1.7107(5) 0.0332(18) Uani 1 1 d . . . H32A H 0.0692 -0.2646 1.6914 0.040 Uiso 1 1 calc R . . C33 C -0.0515(7) -0.3332(6) 1.7996(5) 0.0367(19) Uani 1 1 d . . . H33A H 0.0062 -0.3788 1.8399 0.044 Uiso 1 1 calc R . . C34 C -0.1720(7) -0.3343(6) 1.8289(5) 0.0317(18) Uani 1 1 d . . . C35 C -0.2530(7) -0.2651(6) 1.7684(5) 0.0327(18) Uani 1 1 d . . . H35A H -0.3374 -0.2620 1.7869 0.039 Uiso 1 1 calc R . . C36 C -0.2081(7) -0.2000(6) 1.6801(5) 0.0356(18) Uani 1 1 d . . . H36A H -0.2641 -0.1537 1.6386 0.043 Uiso 1 1 calc R . . N37 N -0.2136(6) -0.4039(5) 1.9199(4) 0.0360(15) Uani 1 1 d . . . C38 C -0.2834(7) -0.4874(7) 1.9271(5) 0.043(2) Uani 1 1 d . . . H38A H -0.3059 -0.5294 1.9930 0.064 Uiso 1 1 calc R . . H38B H -0.2337 -0.5406 1.8946 0.064 Uiso 1 1 calc R . . H38C H -0.3568 -0.4473 1.8986 0.064 Uiso 1 1 calc R . . C39 C -0.1752(7) -0.4124(6) 1.9980(5) 0.0342(18) Uani 1 1 d . . . O40 O -0.1789(5) -0.4967(4) 2.0681(3) 0.0428(14) Uani 1 1 d . . . C41 C -0.1372(7) -0.3142(6) 2.0020(5) 0.0350(18) Uani 1 1 d . . . S42 S -0.18981(18) -0.17580(16) 1.93802(12) 0.0358(5) Uani 1 1 d . . . C43 C -0.1253(7) -0.1255(6) 1.9987(4) 0.0328(18) Uani 1 1 d . . . C44 C -0.0641(7) -0.2126(6) 2.0645(4) 0.0351(18) Uani 1 1 d . . . H44A H -0.0222 -0.2015 2.1047 0.042 Uiso 1 1 calc R . . C45 C -0.0705(7) -0.3201(7) 2.0658(5) 0.0393(19) Uani 1 1 d . . . H45A H -0.0324 -0.3896 2.1066 0.047 Uiso 1 1 calc R . . C46 C -0.1522(6) -0.0037(6) 1.9923(5) 0.0353(18) Uani 1 1 d . . . O47 O -0.1598(5) 0.0213(4) 2.0622(3) 0.0408(13) Uani 1 1 d . . . N48 N -0.1803(6) 0.0795(5) 1.9105(4) 0.0337(15) Uani 1 1 d . . . C49 C -0.2418(7) 0.1950(6) 1.9152(5) 0.0376(19) Uani 1 1 d . . . H49A H -0.2654 0.1920 1.9806 0.056 Uiso 1 1 calc R . . H49B H -0.3140 0.2222 1.8847 0.056 Uiso 1 1 calc R . . H49C H -0.1864 0.2471 1.8834 0.056 Uiso 1 1 calc R . . C50 C -0.1395(7) 0.0676(6) 1.8192(5) 0.0333(18) Uani 1 1 d . . . C51 C -0.0243(7) 0.0124(6) 1.7940(4) 0.0346(18) Uani 1 1 d . . . H51A H 0.0292 -0.0259 1.8389 0.041 Uiso 1 1 calc R . . C52 C 0.0127(7) 0.0129(6) 1.7046(5) 0.0359(19) Uani 1 1 d . . . H52A H 0.0919 -0.0280 1.6893 0.043 Uiso 1 1 calc R . . N53 N -0.0552(6) 0.0671(5) 1.6363(4) 0.0390(16) Uani 1 1 d . . . C54 C -0.1701(8) 0.1197(7) 1.6620(5) 0.044(2) Uani 1 1 d . . . H54A H -0.2223 0.1579 1.6163 0.053 Uiso 1 1 calc R . . C55 C -0.2129(7) 0.1190(6) 1.7523(5) 0.0371(19) Uani 1 1 d . . . H55A H -0.2944 0.1547 1.7682 0.045 Uiso 1 1 calc R . . N60 N 0.2729(6) -0.1072(6) 1.5233(4) 0.0412(16) Uani 1 1 d . . . O61 O 0.1939(5) -0.1655(5) 1.5590(4) 0.0572(17) Uani 1 1 d . . . O62 O 0.3756(5) -0.1522(5) 1.4918(4) 0.0619(17) Uani 1 1 d . . . O63 O 0.2479(5) -0.0050(5) 1.5177(4) 0.0506(15) Uani 1 1 d . . . N70 N 0.8665(6) 0.4417(6) 0.7017(4) 0.0400(16) Uani 1 1 d . . . O71 O 0.8235(6) 0.3784(5) 0.6806(4) 0.0607(17) Uani 1 1 d . . . O72 O 0.8656(5) 0.5416(5) 0.6492(4) 0.0629(18) Uani 1 1 d . . . O73 O 0.9126(5) 0.4057(5) 0.7744(3) 0.0478(14) Uani 1 1 d . . . C81 C 0.2649(8) 0.7416(8) 0.8704(6) 0.065(3) Uani 1 1 d . . . H81A H 0.2233 0.6794 0.9108 0.078 Uiso 1 1 calc R . . H81B H 0.2226 0.8108 0.8875 0.078 Uiso 1 1 calc R . . Cl82 Cl 0.2558(2) 0.7663(2) 0.75634(16) 0.0735(8) Uani 1 1 d . . . Cl83 Cl 0.4197(3) 0.7037(3) 0.89152(18) 0.0834(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0424(4) 0.0371(4) 0.0386(4) -0.0049(3) -0.0153(3) -0.0065(3) Ag2 0.0580(4) 0.0395(4) 0.0253(3) -0.0022(3) 0.0006(3) -0.0191(3) N1 0.039(4) 0.028(4) 0.040(4) -0.003(3) -0.006(3) -0.009(3) C2 0.040(5) 0.027(4) 0.034(4) -0.002(3) -0.002(4) -0.011(4) C3 0.042(5) 0.026(4) 0.037(4) -0.001(3) -0.006(4) -0.008(4) C4 0.046(5) 0.023(4) 0.048(5) -0.004(4) -0.014(4) -0.012(4) C5 0.044(5) 0.027(4) 0.044(5) -0.007(4) -0.011(4) -0.005(4) C6 0.040(5) 0.038(5) 0.031(4) 0.000(4) -0.002(4) -0.011(4) N7 0.045(4) 0.032(4) 0.050(4) -0.003(3) -0.022(3) -0.016(3) C8 0.070(7) 0.035(5) 0.091(7) -0.002(5) -0.029(6) -0.024(5) C9 0.048(5) 0.036(5) 0.061(6) -0.016(4) -0.023(5) -0.010(4) O10 0.088(5) 0.042(4) 0.084(5) -0.013(3) -0.049(4) -0.018(4) C11 0.044(5) 0.046(5) 0.045(5) -0.011(4) -0.020(4) -0.005(4) S12 0.0491(13) 0.0311(11) 0.0400(11) -0.0038(9) -0.0148(10) -0.0103(10) C13 0.046(5) 0.025(4) 0.044(5) 0.002(3) -0.021(4) -0.006(4) C14 0.045(5) 0.053(6) 0.039(5) -0.002(4) -0.016(4) -0.013(4) C15 0.045(5) 0.053(6) 0.027(4) -0.017(4) -0.012(4) -0.005(4) C16 0.051(5) 0.035(5) 0.062(6) -0.013(4) -0.025(5) -0.003(4) O17 0.096(5) 0.033(4) 0.106(5) -0.017(4) -0.069(5) 0.008(4) N18 0.048(4) 0.025(4) 0.046(4) -0.006(3) -0.019(3) 0.000(3) C19 0.065(6) 0.038(5) 0.068(6) -0.020(5) -0.025(5) -0.001(5) C20 0.042(5) 0.021(4) 0.032(4) 0.000(3) -0.019(4) -0.004(3) C21 0.043(5) 0.037(5) 0.032(4) -0.005(4) -0.010(4) -0.014(4) C22 0.040(5) 0.033(4) 0.032(4) -0.003(3) -0.002(4) -0.013(4) N23 0.031(4) 0.033(4) 0.028(3) -0.003(3) -0.005(3) -0.013(3) C24 0.051(5) 0.043(5) 0.032(4) -0.001(4) -0.007(4) -0.019(4) C25 0.047(5) 0.037(5) 0.033(4) -0.012(4) 0.003(4) -0.012(4) N31 0.037(4) 0.034(4) 0.025(3) -0.005(3) -0.001(3) -0.013(3) C32 0.034(4) 0.033(4) 0.032(4) -0.010(3) -0.004(4) -0.008(4) C33 0.048(5) 0.033(4) 0.029(4) -0.008(3) -0.004(4) -0.012(4) C34 0.048(5) 0.024(4) 0.026(4) -0.008(3) -0.003(4) -0.015(4) C35 0.030(4) 0.035(4) 0.032(4) -0.009(3) -0.007(3) -0.007(4) C36 0.041(5) 0.032(4) 0.031(4) -0.001(3) -0.014(4) -0.009(4) N37 0.048(4) 0.032(4) 0.029(3) -0.003(3) -0.009(3) -0.017(3) C38 0.052(5) 0.041(5) 0.042(5) -0.007(4) -0.006(4) -0.030(4) C39 0.034(4) 0.034(5) 0.032(4) 0.000(3) -0.005(3) -0.016(4) O40 0.061(4) 0.031(3) 0.029(3) 0.008(2) -0.008(3) -0.020(3) C41 0.046(5) 0.031(4) 0.023(4) -0.002(3) -0.004(3) -0.009(4) S42 0.0465(12) 0.0298(11) 0.0300(10) 0.0000(8) -0.0114(9) -0.0148(9) C43 0.040(5) 0.032(4) 0.019(4) 0.000(3) 0.002(3) -0.013(4) C44 0.050(5) 0.040(5) 0.020(4) -0.004(3) -0.012(3) -0.019(4) C45 0.051(5) 0.036(5) 0.028(4) 0.000(3) -0.010(4) -0.014(4) C46 0.031(4) 0.038(5) 0.035(4) -0.008(4) -0.004(4) -0.011(4) O47 0.056(4) 0.041(3) 0.028(3) -0.009(2) -0.009(3) -0.015(3) N48 0.045(4) 0.027(3) 0.027(3) 0.000(3) -0.009(3) -0.014(3) C49 0.052(5) 0.032(4) 0.028(4) -0.009(3) -0.010(4) -0.005(4) C50 0.039(5) 0.027(4) 0.031(4) -0.007(3) 0.001(4) -0.012(4) C51 0.038(5) 0.036(4) 0.024(4) 0.002(3) -0.006(3) -0.013(4) C52 0.033(4) 0.041(5) 0.032(4) -0.012(4) 0.001(4) -0.010(4) N53 0.051(4) 0.033(4) 0.025(3) 0.001(3) -0.001(3) -0.016(3) C54 0.062(6) 0.033(5) 0.035(5) -0.005(4) -0.009(4) -0.012(4) C55 0.041(5) 0.036(5) 0.029(4) -0.005(3) -0.011(4) -0.004(4) N60 0.041(4) 0.039(4) 0.041(4) -0.010(3) -0.002(3) -0.012(4) O61 0.054(4) 0.064(4) 0.046(3) -0.002(3) 0.000(3) -0.029(3) O62 0.046(4) 0.055(4) 0.082(4) -0.025(4) 0.008(3) -0.016(3) O63 0.057(4) 0.036(4) 0.052(4) -0.008(3) -0.014(3) -0.003(3) N70 0.041(4) 0.040(4) 0.032(4) -0.007(3) -0.002(3) -0.007(3) O71 0.079(5) 0.065(4) 0.054(4) -0.023(3) -0.007(3) -0.037(4) O72 0.060(4) 0.043(4) 0.056(4) 0.019(3) -0.007(3) -0.012(3) O73 0.057(4) 0.049(4) 0.034(3) 0.002(3) -0.018(3) -0.017(3) C81 0.076(7) 0.051(6) 0.055(6) -0.009(5) -0.007(5) -0.008(5) Cl82 0.0793(18) 0.0806(19) 0.0592(15) -0.0124(13) -0.0148(13) -0.0249(15) Cl83 0.0689(18) 0.112(3) 0.0637(16) -0.0153(16) -0.0051(14) -0.0325(17) _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 2.132(6) . ? Ag1 N23 2.150(6) 2_566 ? Ag1 Ag1 3.1399(13) 2_566 ? Ag2 N53 2.145(6) 2_558 ? Ag2 N31 2.152(5) . ? Ag2 Ag2 3.0378(13) 2_558 ? N1 C6 1.350(9) . ? N1 C2 1.351(8) . ? C2 C3 1.378(10) . ? C2 H2A 0.9500 . ? C3 C4 1.384(10) . ? C3 H3A 0.9500 . ? C4 N7 1.399(9) . ? C4 C5 1.412(10) . ? C5 C6 1.363(10) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N7 C9 1.366(9) . ? N7 C8 1.473(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O10 1.216(9) . ? C9 C11 1.486(11) . ? C11 C15 1.361(10) . ? C11 S12 1.731(8) . ? S12 C13 1.719(7) . ? C13 C14 1.372(10) . ? C13 C16 1.506(11) . ? C14 C15 1.385(11) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 O17 1.216(9) . ? C16 N18 1.375(10) . ? N18 C20 1.411(9) . ? N18 C19 1.480(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.366(9) . ? C20 C21 1.397(10) . ? C21 C22 1.359(10) . ? C21 H21A 0.9500 . ? C22 N23 1.344(8) . ? C22 H22A 0.9500 . ? N23 C24 1.335(9) . ? N23 Ag1 2.150(6) 2_566 ? C24 C25 1.386(10) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N31 C36 1.326(9) . ? N31 C32 1.346(8) . ? C32 C33 1.386(9) . ? C32 H32A 0.9500 . ? C33 C34 1.372(10) . ? C33 H33A 0.9500 . ? C34 C35 1.384(9) . ? C34 N37 1.427(8) . ? C35 C36 1.390(9) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N37 C39 1.353(9) . ? N37 C38 1.481(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O40 1.232(8) . ? C39 C41 1.483(10) . ? C41 C45 1.370(10) . ? C41 S42 1.716(7) . ? S42 C43 1.716(8) . ? C43 C44 1.373(9) . ? C43 C46 1.487(10) . ? C44 C45 1.406(10) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 O47 1.224(8) . ? C46 N48 1.375(8) . ? N48 C50 1.439(9) . ? N48 C49 1.487(9) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.364(9) . ? C50 C51 1.372(10) . ? C51 C52 1.357(9) . ? C51 H51A 0.9500 . ? C52 N53 1.339(9) . ? C52 H52A 0.9500 . ? N53 C54 1.360(10) . ? N53 Ag2 2.145(6) 2_558 ? C54 C55 1.374(10) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? N60 O62 1.245(8) . ? N60 O63 1.246(8) . ? N60 O61 1.248(8) . ? N70 O71 1.239(8) . ? N70 O73 1.247(7) . ? N70 O72 1.250(8) . ? C81 Cl82 1.712(8) . ? C81 Cl83 1.808(9) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N23 167.6(2) . 2_566 ? N1 Ag1 Ag1 99.38(17) . 2_566 ? N23 Ag1 Ag1 92.45(16) 2_566 2_566 ? N53 Ag2 N31 166.3(2) 2_558 . ? N53 Ag2 Ag2 82.66(17) 2_558 2_558 ? N31 Ag2 Ag2 109.87(16) . 2_558 ? C6 N1 C2 116.0(7) . . ? C6 N1 Ag1 120.3(5) . . ? C2 N1 Ag1 122.3(5) . . ? N1 C2 C3 124.0(7) . . ? N1 C2 H2A 118.0 . . ? C3 C2 H2A 118.0 . . ? C2 C3 C4 119.2(7) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 N7 122.1(7) . . ? C3 C4 C5 117.5(7) . . ? N7 C4 C5 120.3(7) . . ? C6 C5 C4 119.1(8) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? N1 C6 C5 124.2(7) . . ? N1 C6 H6A 117.9 . . ? C5 C6 H6A 117.9 . . ? C9 N7 C4 123.8(7) . . ? C9 N7 C8 116.5(6) . . ? C4 N7 C8 119.0(6) . . ? N7 C8 H8A 109.5 . . ? N7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O10 C9 N7 122.8(8) . . ? O10 C9 C11 118.1(7) . . ? N7 C9 C11 118.7(7) . . ? C15 C11 C9 126.7(8) . . ? C15 C11 S12 108.9(6) . . ? C9 C11 S12 123.5(6) . . ? C13 S12 C11 91.9(4) . . ? C14 C13 C16 124.6(7) . . ? C14 C13 S12 111.9(6) . . ? C16 C13 S12 122.7(6) . . ? C13 C14 C15 110.9(7) . . ? C13 C14 H14A 124.6 . . ? C15 C14 H14A 124.6 . . ? C11 C15 C14 116.4(7) . . ? C11 C15 H15A 121.8 . . ? C14 C15 H15A 121.8 . . ? O17 C16 N18 122.2(8) . . ? O17 C16 C13 119.9(7) . . ? N18 C16 C13 117.6(7) . . ? C16 N18 C20 124.5(6) . . ? C16 N18 C19 118.3(6) . . ? C20 N18 C19 117.1(6) . . ? N18 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.8(7) . . ? C25 C20 N18 120.1(7) . . ? C21 C20 N18 121.9(6) . . ? C22 C21 C20 119.1(7) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? N23 C22 C21 123.5(7) . . ? N23 C22 H22A 118.2 . . ? C21 C22 H22A 118.2 . . ? C24 N23 C22 117.3(6) . . ? C24 N23 Ag1 117.3(5) . 2_566 ? C22 N23 Ag1 123.8(5) . 2_566 ? N23 C24 C25 122.4(7) . . ? N23 C24 H24A 118.8 . . ? C25 C24 H24A 118.8 . . ? C20 C25 C24 119.9(7) . . ? C20 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C36 N31 C32 116.7(6) . . ? C36 N31 Ag2 122.3(5) . . ? C32 N31 Ag2 120.5(5) . . ? N31 C32 C33 123.1(7) . . ? N31 C32 H32A 118.5 . . ? C33 C32 H32A 118.5 . . ? C34 C33 C32 119.4(7) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 C35 118.3(7) . . ? C33 C34 N37 121.1(7) . . ? C35 C34 N37 120.6(7) . . ? C34 C35 C36 118.5(7) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? N31 C36 C35 124.0(7) . . ? N31 C36 H36A 118.0 . . ? C35 C36 H36A 118.0 . . ? C39 N37 C34 123.4(6) . . ? C39 N37 C38 117.5(6) . . ? C34 N37 C38 117.9(6) . . ? N37 C38 H38A 109.5 . . ? N37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O40 C39 N37 121.6(7) . . ? O40 C39 C41 119.0(7) . . ? N37 C39 C41 119.2(6) . . ? C45 C41 C39 124.6(7) . . ? C45 C41 S42 111.3(6) . . ? C39 C41 S42 123.5(6) . . ? C43 S42 C41 91.8(4) . . ? C44 C43 C46 124.2(7) . . ? C44 C43 S42 111.5(6) . . ? C46 C43 S42 123.3(5) . . ? C43 C44 C45 112.4(7) . . ? C43 C44 H44A 123.8 . . ? C45 C44 H44A 123.8 . . ? C41 C45 C44 113.0(7) . . ? C41 C45 H45A 123.5 . . ? C44 C45 H45A 123.5 . . ? O47 C46 N48 120.3(7) . . ? O47 C46 C43 119.6(7) . . ? N48 C46 C43 119.7(7) . . ? C46 N48 C50 124.8(6) . . ? C46 N48 C49 117.4(6) . . ? C50 N48 C49 117.2(5) . . ? N48 C49 H49A 109.5 . . ? N48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 117.6(7) . . ? C55 C50 N48 120.1(7) . . ? C51 C50 N48 122.1(7) . . ? C52 C51 C50 119.5(7) . . ? C52 C51 H51A 120.3 . . ? C50 C51 H51A 120.3 . . ? N53 C52 C51 124.3(7) . . ? N53 C52 H52A 117.8 . . ? C51 C52 H52A 117.8 . . ? C52 N53 C54 116.0(6) . . ? C52 N53 Ag2 121.5(5) . 2_558 ? C54 N53 Ag2 120.0(5) . 2_558 ? N53 C54 C55 121.9(7) . . ? N53 C54 H54A 119.1 . . ? C55 C54 H54A 119.1 . . ? C50 C55 C54 120.6(8) . . ? C50 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? O62 N60 O63 120.8(7) . . ? O62 N60 O61 119.0(7) . . ? O63 N60 O61 120.1(7) . . ? O71 N70 O73 120.3(7) . . ? O71 N70 O72 120.0(7) . . ? O73 N70 O72 119.7(7) . . ? Cl82 C81 Cl83 112.3(5) . . ? Cl82 C81 H81A 109.2 . . ? Cl83 C81 H81A 109.2 . . ? Cl82 C81 H81B 109.2 . . ? Cl83 C81 H81B 109.2 . . ? H81A C81 H81B 107.9 . . ? 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 N23 Ag1 N1 C6 -79.0(12) 2_566 . . . ? Ag1 Ag1 N1 C6 119.0(6) 2_566 . . . ? N23 Ag1 N1 C2 86.9(12) 2_566 . . . ? Ag1 Ag1 N1 C2 -75.1(6) 2_566 . . . ? C6 N1 C2 C3 0.4(11) . . . . ? Ag1 N1 C2 C3 -166.0(6) . . . . ? N1 C2 C3 C4 -0.6(12) . . . . ? C2 C3 C4 N7 178.4(7) . . . . ? C2 C3 C4 C5 1.3(11) . . . . ? C3 C4 C5 C6 -1.8(11) . . . . ? N7 C4 C5 C6 -179.0(7) . . . . ? C2 N1 C6 C5 -1.0(11) . . . . ? Ag1 N1 C6 C5 165.7(6) . . . . ? C4 C5 C6 N1 1.7(12) . . . . ? C3 C4 N7 C9 34.0(12) . . . . ? C5 C4 N7 C9 -148.9(8) . . . . ? C3 C4 N7 C8 -137.0(8) . . . . ? C5 C4 N7 C8 40.1(11) . . . . ? C4 N7 C9 O10 -156.0(8) . . . . ? C8 N7 C9 O10 15.2(12) . . . . ? C4 N7 C9 C11 31.6(12) . . . . ? C8 N7 C9 C11 -157.2(8) . . . . ? O10 C9 C11 C15 25.9(14) . . . . ? N7 C9 C11 C15 -161.3(8) . . . . ? O10 C9 C11 S12 -142.0(7) . . . . ? N7 C9 C11 S12 30.9(11) . . . . ? C15 C11 S12 C13 -0.2(7) . . . . ? C9 C11 S12 C13 169.6(7) . . . . ? C11 S12 C13 C14 1.1(7) . . . . ? C11 S12 C13 C16 -169.3(7) . . . . ? C16 C13 C14 C15 168.5(8) . . . . ? S12 C13 C14 C15 -1.7(9) . . . . ? C9 C11 C15 C14 -170.2(8) . . . . ? S12 C11 C15 C14 -0.8(10) . . . . ? C13 C14 C15 C11 1.7(11) . . . . ? C14 C13 C16 O17 -37.3(13) . . . . ? S12 C13 C16 O17 131.9(8) . . . . ? C14 C13 C16 N18 149.5(8) . . . . ? S12 C13 C16 N18 -41.4(11) . . . . ? O17 C16 N18 C20 163.8(9) . . . . ? C13 C16 N18 C20 -23.1(12) . . . . ? O17 C16 N18 C19 -11.6(13) . . . . ? C13 C16 N18 C19 161.5(7) . . . . ? C16 N18 C20 C25 137.8(8) . . . . ? C19 N18 C20 C25 -46.8(10) . . . . ? C16 N18 C20 C21 -46.9(11) . . . . ? C19 N18 C20 C21 128.6(8) . . . . ? C25 C20 C21 C22 1.8(11) . . . . ? N18 C20 C21 C22 -173.7(7) . . . . ? C20 C21 C22 N23 -1.4(12) . . . . ? C21 C22 N23 C24 0.2(11) . . . . ? C21 C22 N23 Ag1 165.3(6) . . . 2_566 ? C22 N23 C24 C25 0.5(11) . . . . ? Ag1 N23 C24 C25 -165.5(6) 2_566 . . . ? C21 C20 C25 C24 -1.1(11) . . . . ? N18 C20 C25 C24 174.5(7) . . . . ? N23 C24 C25 C20 -0.1(12) . . . . ? N53 Ag2 N31 C36 -102.6(11) 2_558 . . . ? Ag2 Ag2 N31 C36 102.3(6) 2_558 . . . ? N53 Ag2 N31 C32 69.6(12) 2_558 . . . ? Ag2 Ag2 N31 C32 -85.5(5) 2_558 . . . ? C36 N31 C32 C33 0.8(11) . . . . ? Ag2 N31 C32 C33 -171.8(5) . . . . ? N31 C32 C33 C34 -0.2(11) . . . . ? C32 C33 C34 C35 -1.0(11) . . . . ? C32 C33 C34 N37 179.7(6) . . . . ? C33 C34 C35 C36 1.7(11) . . . . ? N37 C34 C35 C36 -179.1(6) . . . . ? C32 N31 C36 C35 -0.1(11) . . . . ? Ag2 N31 C36 C35 172.3(5) . . . . ? C34 C35 C36 N31 -1.1(12) . . . . ? C33 C34 N37 C39 44.8(11) . . . . ? C35 C34 N37 C39 -134.4(8) . . . . ? C33 C34 N37 C38 -122.9(8) . . . . ? C35 C34 N37 C38 57.9(9) . . . . ? C34 N37 C39 O40 -155.4(7) . . . . ? C38 N37 C39 O40 12.4(11) . . . . ? C34 N37 C39 C41 29.7(11) . . . . ? C38 N37 C39 C41 -162.6(7) . . . . ? O40 C39 C41 C45 21.4(12) . . . . ? N37 C39 C41 C45 -163.6(7) . . . . ? O40 C39 C41 S42 -148.9(6) . . . . ? N37 C39 C41 S42 26.2(10) . . . . ? C45 C41 S42 C43 -1.3(6) . . . . ? C39 C41 S42 C43 170.1(6) . . . . ? C41 S42 C43 C44 1.0(6) . . . . ? C41 S42 C43 C46 -168.5(6) . . . . ? C46 C43 C44 C45 169.0(7) . . . . ? S42 C43 C44 C45 -0.3(8) . . . . ? C39 C41 C45 C44 -169.9(7) . . . . ? S42 C41 C45 C44 1.4(9) . . . . ? C43 C44 C45 C41 -0.7(10) . . . . ? C44 C43 C46 O47 -26.0(11) . . . . ? S42 C43 C46 O47 142.1(6) . . . . ? C44 C43 C46 N48 160.6(7) . . . . ? S42 C43 C46 N48 -31.3(10) . . . . ? O47 C46 N48 C50 159.0(7) . . . . ? C43 C46 N48 C50 -27.7(11) . . . . ? O47 C46 N48 C49 -11.5(10) . . . . ? C43 C46 N48 C49 161.9(7) . . . . ? C46 N48 C50 C55 145.0(7) . . . . ? C49 N48 C50 C55 -44.5(10) . . . . ? C46 N48 C50 C51 -39.8(11) . . . . ? C49 N48 C50 C51 130.7(7) . . . . ? C55 C50 C51 C52 1.3(11) . . . . ? N48 C50 C51 C52 -174.0(7) . . . . ? C50 C51 C52 N53 2.0(12) . . . . ? C51 C52 N53 C54 -3.3(11) . . . . ? C51 C52 N53 Ag2 158.6(6) . . . 2_558 ? C52 N53 C54 C55 1.4(11) . . . . ? Ag2 N53 C54 C55 -160.8(6) 2_558 . . . ? C51 C50 C55 C54 -3.1(11) . . . . ? N48 C50 C55 C54 172.3(7) . . . . ? N53 C54 C55 C50 1.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.221 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.135 #===END data_8c _database_code_depnum_ccdc_archive 'CCDC 604512' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H38 Ag2 F6 N8 O11 S4' _chemical_formula_weight 1276.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4354(5) _cell_length_b 13.9401(7) _cell_length_c 16.2085(9) _cell_angle_alpha 108.136(2) _cell_angle_beta 97.541(3) _cell_angle_gamma 117.121(2) _cell_volume 2430.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7952 _exptl_absorpt_correction_T_max 0.8782 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19108 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8518 _reflns_number_gt 5516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius 19097-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor. 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1237P)^2^+5.3953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8518 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2305 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.005 _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 0.10120(6) 1.12924(6) 0.49725(4) 0.0567(3) Uani 1 1 d . . . Ag2 Ag 0.37618(6) 1.39020(7) 0.51699(5) 0.0606(3) Uani 1 1 d . . . N1 N 0.1683(6) 1.2501(6) 0.6403(4) 0.0453(16) Uani 1 1 d . . . C2 C 0.1429(7) 1.3324(7) 0.6693(6) 0.049(2) Uani 1 1 d . . . H2A H 0.0843 1.3298 0.6272 0.058 Uiso 1 1 calc R . . C3 C 0.1957(7) 1.4232(7) 0.7571(6) 0.0453(19) Uani 1 1 d . . . H3A H 0.1737 1.4805 0.7749 0.054 Uiso 1 1 calc R . . C4 C 0.2817(6) 1.4268(7) 0.8177(5) 0.0404(18) Uani 1 1 d . . . C5 C 0.3085(6) 1.3401(7) 0.7893(5) 0.0411(18) Uani 1 1 d . . . H5A H 0.3662 1.3402 0.8301 0.049 Uiso 1 1 calc R . . C6 C 0.2505(7) 1.2531(7) 0.7006(5) 0.0428(19) Uani 1 1 d . . . H6A H 0.2690 1.1933 0.6812 0.051 Uiso 1 1 calc R . . N7 N 0.3428(6) 1.5213(6) 0.9073(4) 0.0420(15) Uani 1 1 d . . . C8 C 0.3922(7) 1.6450(7) 0.9164(6) 0.049(2) Uani 1 1 d . . . H8A H 0.4315 1.7004 0.9814 0.073 Uiso 1 1 calc R . . H8B H 0.3282 1.6535 0.8905 0.073 Uiso 1 1 calc R . . H8C H 0.4496 1.6626 0.8833 0.073 Uiso 1 1 calc R . . C9 C 0.3716(7) 1.5071(7) 0.9857(5) 0.0410(18) Uani 1 1 d . . . O10 O 0.4501(5) 1.5901(5) 1.0549(4) 0.0479(14) Uani 1 1 d . . . C11 C 0.2965(7) 1.3913(7) 0.9900(5) 0.0403(18) Uani 1 1 d . . . S12 S 0.14854(17) 1.29526(18) 0.92695(13) 0.0419(5) Uani 1 1 d . . . C13 C 0.1284(7) 1.2179(7) 0.9939(5) 0.0433(19) Uani 1 1 d . . . C14 C 0.2334(7) 1.2635(7) 1.0580(5) 0.0437(19) Uani 1 1 d . . . H14A H 0.2416 1.2310 1.1001 0.052 Uiso 1 1 calc R . . C15 C 0.3271(7) 1.3614(7) 1.0561(6) 0.0454(19) Uani 1 1 d . . . H15A H 0.4051 1.4033 1.0974 0.055 Uiso 1 1 calc R . . C16 C 0.0119(7) 1.1317(7) 0.9919(5) 0.046(2) Uani 1 1 d . . . O17 O 0.0002(6) 1.1225(5) 1.0641(4) 0.0579(16) Uani 1 1 d . . . N18 N -0.0844(6) 1.0766(6) 0.9150(5) 0.0470(17) Uani 1 1 d . . . C19 C -0.2023(8) 1.0315(9) 0.9250(7) 0.061(2) Uani 1 1 d . . . H19A H -0.1946 1.0610 0.9902 0.092 Uiso 1 1 calc R . . H19B H -0.2466 0.9444 0.8973 0.092 Uiso 1 1 calc R . . H19C H -0.2445 1.0589 0.8940 0.092 Uiso 1 1 calc R . . C20 C -0.0767(7) 1.0444(7) 0.8259(5) 0.0415(18) Uani 1 1 d . . . C21 C -0.1460(7) 1.0487(8) 0.7563(6) 0.052(2) Uani 1 1 d . . . H21A H -0.1948 1.0799 0.7691 0.062 Uiso 1 1 calc R . . C22 C -0.1415(8) 1.0068(9) 0.6692(6) 0.057(2) Uani 1 1 d . . . H22A H -0.1893 1.0089 0.6219 0.068 Uiso 1 1 calc R . . N23 N -0.0745(6) 0.9636(6) 0.6472(4) 0.0490(17) Uani 1 1 d . . . C24 C -0.0069(7) 0.9612(7) 0.7129(5) 0.047(2) Uani 1 1 d . . . H24A H 0.0419 0.9307 0.6977 0.057 Uiso 1 1 calc R . . C25 C -0.0053(7) 1.0009(7) 0.8012(5) 0.0427(19) Uani 1 1 d . . . H25A H 0.0453 0.9988 0.8466 0.051 Uiso 1 1 calc R . . N31 N 0.2417(6) 1.3937(6) 0.4309(5) 0.0520(18) Uani 1 1 d . . . C32 C 0.1879(8) 1.4462(8) 0.4697(7) 0.058(2) Uani 1 1 d . . . H32A H 0.2179 1.4908 0.5344 0.070 Uiso 1 1 calc R . . C33 C 0.0917(8) 1.4392(8) 0.4214(6) 0.057(2) Uani 1 1 d . . . H33A H 0.0579 1.4805 0.4520 0.068 Uiso 1 1 calc R . . C34 C 0.0447(7) 1.3727(7) 0.3293(6) 0.0439(19) Uani 1 1 d . . . C35 C 0.1011(7) 1.3200(7) 0.2866(6) 0.0449(19) Uani 1 1 d . . . H35A H 0.0728 1.2761 0.2219 0.054 Uiso 1 1 calc R . . C36 C 0.1981(7) 1.3323(8) 0.3391(6) 0.049(2) Uani 1 1 d . . . H36A H 0.2363 1.2959 0.3095 0.059 Uiso 1 1 calc R . . N37 N -0.0612(6) 1.3566(7) 0.2790(5) 0.0523(18) Uani 1 1 d . . . C38 C -0.1631(8) 1.3123(10) 0.3142(8) 0.071(3) Uani 1 1 d . . . H38A H -0.2314 1.3037 0.2749 0.107 Uiso 1 1 calc R . . H38B H -0.1416 1.3691 0.3770 0.107 Uiso 1 1 calc R . . H38C H -0.1831 1.2350 0.3136 0.107 Uiso 1 1 calc R . . C39 C -0.0845(7) 1.3528(8) 0.1923(7) 0.051(2) Uani 1 1 d . . . O40 O -0.1845(5) 1.3041(6) 0.1431(5) 0.0705(19) Uani 1 1 d . . . C41 C 0.0151(7) 1.4247(7) 0.1657(6) 0.046(2) Uani 1 1 d . . . S42 S 0.13932(19) 1.55784(19) 0.24297(15) 0.0490(5) Uani 1 1 d . . . C43 C 0.1834(7) 1.5915(7) 0.1554(6) 0.047(2) Uani 1 1 d . . . C44 C 0.1066(8) 1.5036(8) 0.0723(6) 0.052(2) Uani 1 1 d . . . H44A H 0.1161 1.5062 0.0158 0.062 Uiso 1 1 calc R . . C45 C 0.0119(8) 1.4088(8) 0.0784(6) 0.052(2) Uani 1 1 d . . . H45A H -0.0488 1.3397 0.0262 0.063 Uiso 1 1 calc R . . C46 C 0.2790(8) 1.7098(9) 0.1695(7) 0.057(2) Uani 1 1 d . . . O47 O 0.2629(7) 1.7534(7) 0.1183(6) 0.092(3) Uani 1 1 d . . . N48 N 0.3795(7) 1.7779(7) 0.2469(6) 0.058(2) Uani 1 1 d . . . C49 C 0.4478(9) 1.9046(10) 0.2717(11) 0.096(5) Uani 1 1 d . . . H49A H 0.4066 1.9240 0.2313 0.144 Uiso 1 1 calc R . . H49B H 0.5258 1.9270 0.2651 0.144 Uiso 1 1 calc R . . H49C H 0.4570 1.9482 0.3355 0.144 Uiso 1 1 calc R . . C50 C 0.4222(7) 1.7308(7) 0.2970(6) 0.045(2) Uani 1 1 d . . . C51 C 0.4876(8) 1.8000(9) 0.3887(7) 0.062(3) Uani 1 1 d . . . H51A H 0.4992 1.8766 0.4177 0.075 Uiso 1 1 calc R . . C52 C 0.5362(8) 1.7588(10) 0.4384(7) 0.069(3) Uani 1 1 d . . . H52A H 0.5795 1.8073 0.5018 0.082 Uiso 1 1 calc R . . N53 N 0.5243(6) 1.6532(7) 0.4004(5) 0.0527(18) Uani 1 1 d . . . C54 C 0.4631(8) 1.5867(9) 0.3115(6) 0.051(2) Uani 1 1 d . . . H54A H 0.4542 1.5111 0.2838 0.062 Uiso 1 1 calc R . . C55 C 0.4122(7) 1.6225(8) 0.2579(6) 0.050(2) Uani 1 1 d . . . H55A H 0.3705 1.5728 0.1945 0.060 Uiso 1 1 calc R . . O61 O 0.4769(8) 1.3692(8) 0.3918(6) 0.095(3) Uani 1 1 d . . . O62 O 0.6168(6) 1.4142(6) 0.3109(5) 0.075(2) Uani 1 1 d . . . O63 O 0.4082(7) 1.2857(7) 0.2289(5) 0.086(2) Uani 1 1 d . . . S64 S 0.5008(2) 1.3305(2) 0.30886(16) 0.0556(6) Uani 1 1 d . . . C65 C 0.5114(9) 1.2084(10) 0.3065(10) 0.076(3) Uani 1 1 d . . . F66 F 0.4132(6) 1.1273(7) 0.3133(7) 0.123(3) Uani 1 1 d . . . F67 F 0.5996(6) 1.2357(8) 0.3728(7) 0.127(3) Uani 1 1 d . . . F68 F 0.5275(7) 1.1569(6) 0.2317(7) 0.121(3) Uani 1 1 d . . . O71 O 0.1816(9) 0.9925(7) 0.5339(5) 0.093(3) Uani 1 1 d . . . O72 O 0.0622(6) 0.8059(7) 0.5391(5) 0.082(2) Uani 1 1 d . . . O73 O 0.2595(6) 0.9400(6) 0.6423(4) 0.0703(18) Uani 1 1 d . . . S74 S 0.1780(2) 0.9010(2) 0.55585(15) 0.0540(6) Uani 1 1 d . . . C75 C 0.2301(11) 0.8318(10) 0.4736(9) 0.081(3) Uani 1 1 d . . . F76 F 0.1617(9) 0.7941(7) 0.3864(5) 0.123(3) Uani 1 1 d . . . F77 F 0.2255(7) 0.7387(7) 0.4786(5) 0.102(2) Uani 1 1 d . . . F78 F 0.3362(9) 0.9071(8) 0.4789(8) 0.171(5) Uani 1 1 d . . . C81 C -0.3884(10) 0.9923(11) 0.0764(10) 0.086(4) Uani 1 1 d . . . H81A H -0.3582 1.0727 0.0802 0.130 Uiso 1 1 calc R . . H81B H -0.4561 0.9690 0.0991 0.130 Uiso 1 1 calc R . . H81C H -0.4133 0.9367 0.0125 0.130 Uiso 1 1 calc R . . C82 C -0.2913(11) 0.9900(13) 0.1350(8) 0.086(4) Uani 1 1 d . . . C83 C -0.3191(9) 0.8802(8) 0.1393(8) 0.074(3) Uani 1 1 d . . . H83A H -0.2505 0.8918 0.1807 0.112 Uiso 1 1 calc R . . H83B H -0.3397 0.8207 0.0779 0.112 Uiso 1 1 calc R . . H83C H -0.3862 0.8528 0.1623 0.112 Uiso 1 1 calc R . . O84 O -0.1875(8) 1.0733(8) 0.1658(7) 0.102(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 0.0636(5) 0.0642(5) 0.0191(3) 0.0107(3) -0.0016(3) 0.0247(4) Ag2 0.0556(4) 0.0863(6) 0.0406(4) 0.0344(4) 0.0028(3) 0.0364(4) N1 0.048(4) 0.052(4) 0.017(3) 0.009(3) -0.003(3) 0.019(3) C2 0.048(5) 0.050(5) 0.031(5) 0.016(4) -0.002(4) 0.018(4) C3 0.047(4) 0.044(4) 0.032(5) 0.012(4) -0.002(4) 0.019(4) C4 0.040(4) 0.041(4) 0.026(4) 0.013(3) 0.005(3) 0.012(3) C5 0.040(4) 0.056(5) 0.020(4) 0.013(3) 0.003(3) 0.024(4) C6 0.050(5) 0.053(5) 0.020(4) 0.012(4) 0.010(3) 0.025(4) N7 0.047(4) 0.042(4) 0.025(4) 0.013(3) 0.002(3) 0.018(3) C8 0.050(5) 0.044(5) 0.039(5) 0.014(4) 0.003(4) 0.019(4) C9 0.041(4) 0.049(5) 0.028(4) 0.014(4) 0.005(4) 0.022(4) O10 0.046(3) 0.051(3) 0.025(3) 0.009(3) -0.004(2) 0.018(3) C11 0.042(4) 0.046(4) 0.030(4) 0.016(4) 0.009(3) 0.022(4) S12 0.0423(11) 0.0476(11) 0.0252(10) 0.0154(9) 0.0016(8) 0.0181(9) C13 0.056(5) 0.051(5) 0.020(4) 0.014(3) 0.007(3) 0.029(4) C14 0.064(5) 0.046(5) 0.019(4) 0.014(3) 0.004(4) 0.030(4) C15 0.053(5) 0.054(5) 0.026(4) 0.017(4) 0.002(4) 0.029(4) C16 0.058(5) 0.049(5) 0.021(4) 0.018(4) 0.004(4) 0.021(4) O17 0.073(4) 0.054(3) 0.027(3) 0.020(3) 0.010(3) 0.018(3) N18 0.048(4) 0.050(4) 0.035(4) 0.016(3) 0.012(3) 0.022(3) C19 0.056(6) 0.073(6) 0.047(6) 0.030(5) 0.022(5) 0.023(5) C20 0.039(4) 0.045(4) 0.021(4) 0.011(3) 0.000(3) 0.012(4) C21 0.045(5) 0.074(6) 0.035(5) 0.025(4) 0.007(4) 0.031(4) C22 0.052(5) 0.076(6) 0.030(5) 0.022(4) -0.001(4) 0.027(5) N23 0.052(4) 0.054(4) 0.021(4) 0.010(3) 0.000(3) 0.019(3) C24 0.057(5) 0.049(5) 0.023(4) 0.013(4) 0.002(4) 0.023(4) C25 0.053(5) 0.040(4) 0.022(4) 0.012(3) -0.001(3) 0.019(4) N31 0.047(4) 0.064(5) 0.039(4) 0.022(4) 0.004(3) 0.027(4) C32 0.058(5) 0.070(6) 0.037(5) 0.013(5) 0.007(4) 0.035(5) C33 0.052(5) 0.076(6) 0.030(5) 0.013(4) 0.008(4) 0.033(5) C34 0.044(4) 0.049(5) 0.038(5) 0.020(4) 0.010(4) 0.025(4) C35 0.048(5) 0.048(5) 0.026(4) 0.012(4) -0.001(3) 0.022(4) C36 0.050(5) 0.057(5) 0.042(5) 0.022(4) 0.013(4) 0.031(4) N37 0.042(4) 0.064(5) 0.053(5) 0.029(4) 0.012(3) 0.028(3) C38 0.053(6) 0.099(8) 0.076(8) 0.049(7) 0.028(5) 0.041(6) C39 0.043(5) 0.060(5) 0.050(6) 0.027(5) 0.003(4) 0.028(4) O40 0.045(4) 0.086(5) 0.064(5) 0.034(4) -0.008(3) 0.028(3) C41 0.045(4) 0.055(5) 0.038(5) 0.019(4) 0.003(4) 0.030(4) S42 0.0526(12) 0.0496(12) 0.0321(12) 0.0144(9) 0.0035(9) 0.0219(10) C43 0.052(5) 0.055(5) 0.039(5) 0.024(4) 0.007(4) 0.032(4) C44 0.068(6) 0.069(6) 0.029(5) 0.026(4) 0.008(4) 0.042(5) C45 0.057(5) 0.050(5) 0.030(5) 0.004(4) -0.007(4) 0.028(4) C46 0.050(5) 0.074(6) 0.050(6) 0.042(5) 0.006(4) 0.028(5) O47 0.078(5) 0.091(5) 0.104(7) 0.070(5) 0.005(4) 0.031(4) N48 0.058(5) 0.057(5) 0.063(6) 0.034(4) 0.013(4) 0.030(4) C49 0.054(6) 0.070(7) 0.151(14) 0.072(8) 0.006(7) 0.014(5) C50 0.040(4) 0.049(5) 0.042(5) 0.027(4) 0.005(4) 0.016(4) C51 0.061(6) 0.058(6) 0.059(7) 0.016(5) 0.001(5) 0.035(5) C52 0.059(6) 0.079(7) 0.047(6) 0.012(5) -0.002(5) 0.035(5) N53 0.052(4) 0.068(5) 0.045(5) 0.030(4) 0.013(3) 0.034(4) C54 0.059(5) 0.072(6) 0.034(5) 0.027(4) 0.011(4) 0.042(5) C55 0.056(5) 0.066(6) 0.037(5) 0.025(4) 0.013(4) 0.038(4) O61 0.105(6) 0.131(7) 0.062(5) 0.033(5) 0.038(5) 0.074(6) O62 0.072(4) 0.066(4) 0.060(5) 0.032(4) 0.011(4) 0.016(4) O63 0.082(5) 0.109(6) 0.047(4) 0.022(4) -0.020(4) 0.052(4) S64 0.0627(14) 0.0711(15) 0.0354(13) 0.0218(11) 0.0056(10) 0.0400(12) C65 0.043(6) 0.072(7) 0.102(10) 0.041(7) 0.014(6) 0.022(5) F66 0.078(5) 0.096(5) 0.195(10) 0.089(6) 0.037(5) 0.031(4) F67 0.069(4) 0.150(7) 0.205(10) 0.130(7) 0.025(5) 0.060(4) F68 0.113(6) 0.088(5) 0.147(9) 0.016(5) 0.039(6) 0.065(5) O71 0.168(8) 0.093(5) 0.049(5) 0.036(4) 0.037(5) 0.087(6) O72 0.054(4) 0.092(5) 0.060(5) 0.018(4) -0.003(3) 0.023(4) O73 0.064(4) 0.087(5) 0.035(4) 0.017(3) -0.002(3) 0.032(4) S74 0.0606(14) 0.0618(14) 0.0278(11) 0.0132(10) 0.0009(10) 0.0307(12) C75 0.089(8) 0.056(6) 0.062(8) 0.000(6) 0.015(6) 0.030(6) F76 0.225(10) 0.102(5) 0.050(4) 0.019(4) 0.043(5) 0.102(6) F77 0.144(6) 0.098(5) 0.079(5) 0.025(4) 0.019(4) 0.087(5) F78 0.135(7) 0.114(6) 0.192(11) 0.005(6) 0.115(8) 0.034(6) C81 0.075(7) 0.100(9) 0.100(10) 0.056(8) 0.047(7) 0.044(7) C82 0.066(7) 0.112(10) 0.051(7) 0.024(7) 0.018(6) 0.033(7) C83 0.070(6) 0.034(5) 0.077(8) -0.004(5) -0.007(5) 0.021(4) O84 0.093(6) 0.103(6) 0.110(8) 0.046(6) 0.035(6) 0.051(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.160(6) . ? Ag1 N23 2.181(7) 2_576 ? Ag2 N31 2.162(7) . ? Ag2 N53 2.172(7) 2_686 ? Ag2 O61 2.597(8) . ? N1 C2 1.310(11) . ? N1 C6 1.350(10) . ? C2 C3 1.388(12) . ? C2 H2A 0.9500 . ? C3 C4 1.386(11) . ? C3 H3A 0.9500 . ? C4 C5 1.377(11) . ? C4 N7 1.424(10) . ? C5 C6 1.380(11) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N7 C9 1.379(10) . ? N7 C8 1.486(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O10 1.216(9) . ? C9 C11 1.494(11) . ? C11 C15 1.344(11) . ? C11 S12 1.726(8) . ? S12 C13 1.719(8) . ? C13 C14 1.364(11) . ? C13 C16 1.464(12) . ? C14 C15 1.385(12) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 O17 1.239(9) . ? C16 N18 1.375(10) . ? N18 C20 1.406(10) . ? N18 C19 1.468(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.389(12) . ? C20 C21 1.401(11) . ? C21 C22 1.371(13) . ? C21 H21A 0.9500 . ? C22 N23 1.321(12) . ? C22 H22A 0.9500 . ? N23 C24 1.325(10) . ? N23 Ag1 2.181(7) 2_576 ? C24 C25 1.358(11) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N31 C32 1.330(12) . ? N31 C36 1.345(11) . ? C32 C33 1.365(13) . ? C32 H32A 0.9500 . ? C33 C34 1.358(12) . ? C33 H33A 0.9500 . ? C34 C35 1.385(12) . ? C34 N37 1.425(10) . ? C35 C36 1.366(11) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N37 C39 1.378(12) . ? N37 C38 1.495(12) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O40 1.205(10) . ? C39 C41 1.475(12) . ? C41 C45 1.355(12) . ? C41 S42 1.726(8) . ? S42 C43 1.722(9) . ? C43 C44 1.355(12) . ? C43 C46 1.476(12) . ? C44 C45 1.400(12) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 O47 1.222(10) . ? C46 N48 1.393(12) . ? N48 C50 1.404(11) . ? N48 C49 1.451(12) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.377(12) . ? C50 C51 1.379(13) . ? C51 C52 1.378(14) . ? C51 H51A 0.9500 . ? C52 N53 1.329(13) . ? C52 H52A 0.9500 . ? N53 C54 1.332(11) . ? N53 Ag2 2.172(7) 2_686 ? C54 C55 1.378(11) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? O61 S64 1.422(8) . ? O62 S64 1.448(7) . ? O63 S64 1.407(7) . ? S64 C65 1.761(12) . ? C65 F68 1.304(15) . ? C65 F67 1.305(13) . ? C65 F66 1.337(12) . ? O71 S74 1.409(8) . ? O72 S74 1.428(7) . ? O73 S74 1.428(7) . ? S74 C75 1.805(12) . ? C75 F78 1.299(13) . ? C75 F77 1.299(13) . ? C75 F76 1.369(15) . ? C81 C82 1.529(17) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 O84 1.233(13) . ? C82 C83 1.429(16) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? 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 N23 166.5(3) . 2_576 ? N31 Ag2 N53 166.3(3) . 2_686 ? N31 Ag2 O61 92.3(3) . . ? N53 Ag2 O61 93.3(3) 2_686 . ? C2 N1 C6 117.6(7) . . ? C2 N1 Ag1 121.5(5) . . ? C6 N1 Ag1 120.3(6) . . ? N1 C2 C3 124.5(8) . . ? N1 C2 H2A 117.7 . . ? C3 C2 H2A 117.7 . . ? C4 C3 C2 117.3(8) . . ? C4 C3 H3A 121.3 . . ? C2 C3 H3A 121.4 . . ? C5 C4 C3 119.2(7) . . ? C5 C4 N7 121.1(7) . . ? C3 C4 N7 119.7(7) . . ? C4 C5 C6 119.1(7) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? N1 C6 C5 122.3(8) . . ? N1 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C9 N7 C4 124.1(7) . . ? C9 N7 C8 117.1(6) . . ? C4 N7 C8 118.3(7) . . ? N7 C8 H8A 109.5 . . ? N7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O10 C9 N7 121.4(7) . . ? O10 C9 C11 118.6(7) . . ? N7 C9 C11 119.7(7) . . ? C15 C11 C9 124.2(7) . . ? C15 C11 S12 111.0(6) . . ? C9 C11 S12 123.3(6) . . ? C13 S12 C11 91.6(4) . . ? C14 C13 C16 125.7(7) . . ? C14 C13 S12 110.0(6) . . ? C16 C13 S12 123.3(6) . . ? C13 C14 C15 114.0(7) . . ? C13 C14 H14A 123.0 . . ? C15 C14 H14A 123.0 . . ? C11 C15 C14 113.3(7) . . ? C11 C15 H15A 123.4 . . ? C14 C15 H15A 123.4 . . ? O17 C16 N18 121.2(8) . . ? O17 C16 C13 118.3(7) . . ? N18 C16 C13 119.7(7) . . ? C16 N18 C20 122.3(7) . . ? C16 N18 C19 118.7(7) . . ? C20 N18 C19 118.1(7) . . ? N18 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 116.7(7) . . ? C25 C20 N18 122.0(7) . . ? C21 C20 N18 121.3(8) . . ? C22 C21 C20 118.3(8) . . ? C22 C21 H21A 120.8 . . ? C20 C21 H21A 120.8 . . ? N23 C22 C21 123.7(8) . . ? N23 C22 H22A 118.1 . . ? C21 C22 H22A 118.1 . . ? C22 N23 C24 118.5(8) . . ? C22 N23 Ag1 119.1(6) . 2_576 ? C24 N23 Ag1 121.5(6) . 2_576 ? N23 C24 C25 122.1(8) . . ? N23 C24 H24A 119.0 . . ? C25 C24 H24A 119.0 . . ? C24 C25 C20 120.7(8) . . ? C24 C25 H25A 119.6 . . ? C20 C25 H25A 119.6 . . ? C32 N31 C36 117.0(7) . . ? C32 N31 Ag2 119.3(6) . . ? C36 N31 Ag2 123.2(6) . . ? N31 C32 C33 123.4(9) . . ? N31 C32 H32A 118.3 . . ? C33 C32 H32A 118.3 . . ? C34 C33 C32 119.4(9) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 C35 118.4(8) . . ? C33 C34 N37 120.1(8) . . ? C35 C34 N37 121.5(7) . . ? C36 C35 C34 118.9(8) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? N31 C36 C35 122.8(8) . . ? N31 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? C39 N37 C34 125.1(7) . . ? C39 N37 C38 117.5(7) . . ? C34 N37 C38 115.7(7) . . ? N37 C38 H38A 109.5 . . ? N37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O40 C39 N37 121.0(8) . . ? O40 C39 C41 119.8(8) . . ? N37 C39 C41 118.5(7) . . ? C45 C41 C39 124.9(8) . . ? C45 C41 S42 110.8(7) . . ? C39 C41 S42 123.2(7) . . ? C43 S42 C41 91.4(4) . . ? C44 C43 C46 124.1(8) . . ? C44 C43 S42 111.3(7) . . ? C46 C43 S42 123.6(7) . . ? C43 C44 C45 112.9(8) . . ? C43 C44 H44A 123.6 . . ? C45 C44 H44A 123.6 . . ? C41 C45 C44 113.6(8) . . ? C41 C45 H45A 123.2 . . ? C44 C45 H45A 123.2 . . ? O47 C46 N48 119.8(9) . . ? O47 C46 C43 118.9(8) . . ? N48 C46 C43 120.8(7) . . ? C46 N48 C50 124.3(7) . . ? C46 N48 C49 116.6(8) . . ? C50 N48 C49 118.9(8) . . ? N48 C49 H49A 109.5 . . ? N48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 117.0(8) . . ? C55 C50 N48 123.5(8) . . ? C51 C50 N48 119.1(8) . . ? C52 C51 C50 120.5(9) . . ? C52 C51 H51A 119.7 . . ? C50 C51 H51A 119.7 . . ? N53 C52 C51 121.9(9) . . ? N53 C52 H52A 119.0 . . ? C51 C52 H52A 119.0 . . ? C52 N53 C54 118.0(8) . . ? C52 N53 Ag2 117.6(6) . 2_686 ? C54 N53 Ag2 123.9(6) . 2_686 ? N53 C54 C55 123.0(9) . . ? N53 C54 H54A 118.5 . . ? C55 C54 H54A 118.5 . . ? C50 C55 C54 119.5(9) . . ? C50 C55 H55A 120.3 . . ? C54 C55 H55A 120.3 . . ? S64 O61 Ag2 164.4(6) . . ? O63 S64 O61 114.3(5) . . ? O63 S64 O62 114.9(5) . . ? O61 S64 O62 113.1(5) . . ? O63 S64 C65 105.5(5) . . ? O61 S64 C65 104.0(6) . . ? O62 S64 C65 103.4(5) . . ? F68 C65 F67 104.5(10) . . ? F68 C65 F66 108.1(10) . . ? F67 C65 F66 106.7(10) . . ? F68 C65 S64 112.7(9) . . ? F67 C65 S64 114.0(9) . . ? F66 C65 S64 110.3(8) . . ? O71 S74 O72 114.8(6) . . ? O71 S74 O73 115.2(5) . . ? O72 S74 O73 113.3(5) . . ? O71 S74 C75 104.7(6) . . ? O72 S74 C75 103.2(5) . . ? O73 S74 C75 103.7(5) . . ? F78 C75 F77 110.0(12) . . ? F78 C75 F76 104.7(12) . . ? F77 C75 F76 106.1(8) . . ? F78 C75 S74 111.6(8) . . ? F77 C75 S74 114.0(9) . . ? F76 C75 S74 109.8(9) . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O84 C82 C83 119.5(12) . . ? O84 C82 C81 121.7(12) . . ? C83 C82 C81 117.8(10) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 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 N23 Ag1 N1 C2 98.2(13) 2_576 . . . ? N23 Ag1 N1 C6 -72.9(14) 2_576 . . . ? C6 N1 C2 C3 0.8(12) . . . . ? Ag1 N1 C2 C3 -170.5(7) . . . . ? N1 C2 C3 C4 0.5(13) . . . . ? C2 C3 C4 C5 -1.5(11) . . . . ? C2 C3 C4 N7 177.0(7) . . . . ? C3 C4 C5 C6 1.1(11) . . . . ? N7 C4 C5 C6 -177.3(7) . . . . ? C2 N1 C6 C5 -1.2(11) . . . . ? Ag1 N1 C6 C5 170.2(6) . . . . ? C4 C5 C6 N1 0.2(12) . . . . ? C5 C4 N7 C9 -41.9(11) . . . . ? C3 C4 N7 C9 139.6(8) . . . . ? C5 C4 N7 C8 130.0(8) . . . . ? C3 C4 N7 C8 -48.4(10) . . . . ? C4 N7 C9 O10 158.9(8) . . . . ? C8 N7 C9 O10 -13.1(11) . . . . ? C4 N7 C9 C11 -28.2(11) . . . . ? C8 N7 C9 C11 159.7(7) . . . . ? O10 C9 C11 C15 -18.5(12) . . . . ? N7 C9 C11 C15 168.4(8) . . . . ? O10 C9 C11 S12 146.2(7) . . . . ? N7 C9 C11 S12 -26.8(10) . . . . ? C15 C11 S12 C13 1.9(7) . . . . ? C9 C11 S12 C13 -164.6(7) . . . . ? C11 S12 C13 C14 -2.5(7) . . . . ? C11 S12 C13 C16 167.1(7) . . . . ? C16 C13 C14 C15 -166.7(8) . . . . ? S12 C13 C14 C15 2.6(9) . . . . ? C9 C11 C15 C14 165.6(7) . . . . ? S12 C11 C15 C14 -0.8(9) . . . . ? C13 C14 C15 C11 -1.2(11) . . . . ? C14 C13 C16 O17 21.6(13) . . . . ? S12 C13 C16 O17 -146.3(7) . . . . ? C14 C13 C16 N18 -168.1(8) . . . . ? S12 C13 C16 N18 24.0(11) . . . . ? O17 C16 N18 C20 -154.1(8) . . . . ? C13 C16 N18 C20 35.9(12) . . . . ? O17 C16 N18 C19 15.0(12) . . . . ? C13 C16 N18 C19 -155.0(8) . . . . ? C16 N18 C20 C25 37.8(11) . . . . ? C19 N18 C20 C25 -131.4(8) . . . . ? C16 N18 C20 C21 -145.7(8) . . . . ? C19 N18 C20 C21 45.1(11) . . . . ? C25 C20 C21 C22 2.0(12) . . . . ? N18 C20 C21 C22 -174.6(8) . . . . ? C20 C21 C22 N23 -0.8(14) . . . . ? C21 C22 N23 C24 -0.5(13) . . . . ? C21 C22 N23 Ag1 168.7(7) . . . 2_576 ? C22 N23 C24 C25 0.4(12) . . . . ? Ag1 N23 C24 C25 -168.5(6) 2_576 . . . ? N23 C24 C25 C20 1.0(12) . . . . ? C21 C20 C25 C24 -2.1(11) . . . . ? N18 C20 C25 C24 174.5(7) . . . . ? N53 Ag2 N31 C32 90.8(14) 2_686 . . . ? O61 Ag2 N31 C32 -155.2(7) . . . . ? N53 Ag2 N31 C36 -80.4(15) 2_686 . . . ? O61 Ag2 N31 C36 33.6(7) . . . . ? C36 N31 C32 C33 0.8(13) . . . . ? Ag2 N31 C32 C33 -171.0(7) . . . . ? N31 C32 C33 C34 2.1(15) . . . . ? C32 C33 C34 C35 -4.0(13) . . . . ? C32 C33 C34 N37 174.9(8) . . . . ? C33 C34 C35 C36 3.0(12) . . . . ? N37 C34 C35 C36 -175.8(7) . . . . ? C32 N31 C36 C35 -1.8(12) . . . . ? Ag2 N31 C36 C35 169.6(6) . . . . ? C34 C35 C36 N31 -0.1(13) . . . . ? C33 C34 N37 C39 142.4(9) . . . . ? C35 C34 N37 C39 -38.7(12) . . . . ? C33 C34 N37 C38 -52.8(11) . . . . ? C35 C34 N37 C38 126.1(9) . . . . ? C34 N37 C39 O40 156.9(8) . . . . ? C38 N37 C39 O40 -7.7(13) . . . . ? C34 N37 C39 C41 -32.3(12) . . . . ? C38 N37 C39 C41 163.2(8) . . . . ? O40 C39 C41 C45 -26.2(13) . . . . ? N37 C39 C41 C45 162.8(8) . . . . ? O40 C39 C41 S42 140.2(8) . . . . ? N37 C39 C41 S42 -30.7(11) . . . . ? C45 C41 S42 C43 1.3(7) . . . . ? C39 C41 S42 C43 -166.8(7) . . . . ? C41 S42 C43 C44 -0.7(7) . . . . ? C41 S42 C43 C46 168.3(7) . . . . ? C46 C43 C44 C45 -169.0(8) . . . . ? S42 C43 C44 C45 0.0(10) . . . . ? C39 C41 C45 C44 166.3(8) . . . . ? S42 C41 C45 C44 -1.6(9) . . . . ? C43 C44 C45 C41 1.1(11) . . . . ? C44 C43 C46 O47 33.6(15) . . . . ? S42 C43 C46 O47 -134.1(9) . . . . ? C44 C43 C46 N48 -155.2(9) . . . . ? S42 C43 C46 N48 37.2(12) . . . . ? O47 C46 N48 C50 -163.3(10) . . . . ? C43 C46 N48 C50 25.4(14) . . . . ? O47 C46 N48 C49 11.7(15) . . . . ? C43 C46 N48 C49 -159.5(10) . . . . ? C46 N48 C50 C55 32.9(13) . . . . ? C49 N48 C50 C55 -142.1(10) . . . . ? C46 N48 C50 C51 -153.4(9) . . . . ? C49 N48 C50 C51 31.6(13) . . . . ? C55 C50 C51 C52 -2.4(14) . . . . ? N48 C50 C51 C52 -176.5(9) . . . . ? C50 C51 C52 N53 1.3(16) . . . . ? C51 C52 N53 C54 -0.1(14) . . . . ? C51 C52 N53 Ag2 172.5(8) . . . 2_686 ? C52 N53 C54 C55 0.0(13) . . . . ? Ag2 N53 C54 C55 -172.1(6) 2_686 . . . ? C51 C50 C55 C54 2.3(12) . . . . ? N48 C50 C55 C54 176.1(8) . . . . ? N53 C54 C55 C50 -1.1(13) . . . . ? N31 Ag2 O61 S64 -56(2) . . . . ? N53 Ag2 O61 S64 112(2) 2_686 . . . ? Ag2 O61 S64 O63 37(2) . . . . ? Ag2 O61 S64 O62 171(2) . . . . ? Ag2 O61 S64 C65 -77(2) . . . . ? O63 S64 C65 F68 56.1(9) . . . . ? O61 S64 C65 F68 176.7(8) . . . . ? O62 S64 C65 F68 -65.0(9) . . . . ? O63 S64 C65 F67 175.1(9) . . . . ? O61 S64 C65 F67 -64.3(10) . . . . ? O62 S64 C65 F67 54.1(11) . . . . ? O63 S64 C65 F66 -64.9(11) . . . . ? O61 S64 C65 F66 55.8(11) . . . . ? O62 S64 C65 F66 174.1(9) . . . . ? O71 S74 C75 F78 59.2(12) . . . . ? O72 S74 C75 F78 179.7(11) . . . . ? O73 S74 C75 F78 -61.9(12) . . . . ? O71 S74 C75 F77 -175.4(9) . . . . ? O72 S74 C75 F77 -54.9(10) . . . . ? O73 S74 C75 F77 63.5(10) . . . . ? O71 S74 C75 F76 -56.5(9) . . . . ? O72 S74 C75 F76 64.0(9) . . . . ? O73 S74 C75 F76 -177.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.721 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.152 #===END data_8d _database_code_depnum_ccdc_archive 'CCDC 604513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Ag Cl4 F6 N4 O2 P S' _chemical_formula_weight 775.10 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5598(3) _cell_length_b 19.7777(5) _cell_length_c 12.8335(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.256(2) _cell_angle_gamma 90.00 _cell_volume 2769.93(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description petal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4387 _exptl_absorpt_correction_T_max 0.7096 _exptl_absorpt_process_details 'DENZO-SMN; Otwinowski & Minor,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28876 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4883 _reflns_number_gt 3747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0776P)^2^+5.1142P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4883 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Ag Ag 0.08922(4) 0.162824(17) 0.65223(3) 0.03925(17) Uani 1 1 d . . . N11 N 0.0893(3) 0.26987(18) 0.6712(3) 0.0306(9) Uani 1 1 d . . . C12 C 0.0457(6) 0.2978(2) 0.7470(5) 0.0476(14) Uani 1 1 d . . . H12A H 0.0189 0.2683 0.7929 0.057 Uiso 1 1 calc R . . C13 C 0.0379(5) 0.3653(3) 0.7616(5) 0.0448(13) Uani 1 1 d . . . H13A H 0.0075 0.3816 0.8172 0.054 Uiso 1 1 calc R . . C14 C 0.0745(4) 0.4114(2) 0.6952(3) 0.0258(9) Uani 1 1 d . . . C15 C 0.1202(4) 0.3827(2) 0.6183(4) 0.0297(10) Uani 1 1 d . . . H15A H 0.1481 0.4110 0.5716 0.036 Uiso 1 1 calc R . . C16 C 0.1252(4) 0.3138(2) 0.6092(4) 0.0311(10) Uani 1 1 d . . . H16A H 0.1565 0.2961 0.5549 0.037 Uiso 1 1 calc R . . N17 N 0.0646(3) 0.48088(17) 0.7136(3) 0.0255(8) Uani 1 1 d . . . C18 C 0.0348(5) 0.5005(2) 0.8123(4) 0.0399(12) Uani 1 1 d . . . H18D H 0.0425 0.5496 0.8220 0.060 Uiso 1 1 calc R . . H18E H 0.0915 0.4781 0.8773 0.060 Uiso 1 1 calc R . . H18F H -0.0493 0.4868 0.8035 0.060 Uiso 1 1 calc R . . C19 C 0.0929(4) 0.5298(2) 0.6478(4) 0.0324(11) Uani 1 1 d . . . O20 O 0.1452(4) 0.51761(17) 0.5820(3) 0.0534(11) Uani 1 1 d . . . C21 C 0.0569(4) 0.6007(2) 0.6601(4) 0.0282(10) Uani 1 1 d . . . S22 S 0.15105(10) 0.66248(5) 0.63644(10) 0.0291(3) Uani 1 1 d . . . C23 C 0.0595(4) 0.7258(2) 0.6585(3) 0.0272(10) Uani 1 1 d . . . C24 C -0.0415(4) 0.6998(2) 0.6775(4) 0.0293(10) Uani 1 1 d . . . H24A H -0.1039 0.7268 0.6894 0.035 Uiso 1 1 calc R . . C25 C -0.0427(4) 0.6286(2) 0.6775(4) 0.0301(10) Uani 1 1 d . . . H25A H -0.1068 0.6027 0.6886 0.036 Uiso 1 1 calc R . . C26 C 0.0929(4) 0.7968(2) 0.6412(4) 0.0293(10) Uani 1 1 d . . . O27 O 0.1259(4) 0.80922(17) 0.5631(3) 0.0464(9) Uani 1 1 d . . . N28 N 0.0806(3) 0.84459(17) 0.7154(3) 0.0279(8) Uani 1 1 d . . . C29 C 0.0590(5) 0.8244(2) 0.8180(4) 0.0378(12) Uani 1 1 d . . . H29A H 0.0599 0.7750 0.8234 0.057 Uiso 1 1 calc R . . H29B H -0.0208 0.8415 0.8172 0.057 Uiso 1 1 calc R . . H29C H 0.1236 0.8433 0.8815 0.057 Uiso 1 1 calc R . . C30 C 0.0819(4) 0.9147(2) 0.6941(4) 0.0254(9) Uani 1 1 d . . . C31 C 0.0300(5) 0.9589(3) 0.7503(4) 0.0415(12) Uani 1 1 d . . . H31A H -0.0075 0.9416 0.8004 0.050 Uiso 1 1 calc R . . C32 C 0.0326(5) 1.0267(2) 0.7338(5) 0.0431(13) Uani 1 1 d . . . H32A H -0.0030 1.0556 0.7741 0.052 Uiso 1 1 calc R . . N33 N 0.0826(3) 1.05507(18) 0.6638(3) 0.0319(9) Uani 1 1 d . . . C34 C 0.1319(4) 1.0127(2) 0.6092(4) 0.0350(11) Uani 1 1 d . . . H34A H 0.1680 1.0313 0.5589 0.042 Uiso 1 1 calc R . . C35 C 0.1333(4) 0.9438(2) 0.6219(4) 0.0322(10) Uani 1 1 d . . . H35A H 0.1697 0.9160 0.5808 0.039 Uiso 1 1 calc R . . P40 P 0.30439(12) 1.15692(6) 1.45546(10) 0.0335(3) Uani 1 1 d . . . F41 F 0.4404(4) 1.1644(3) 1.4600(5) 0.121(2) Uani 1 1 d . . . F42 F 0.1678(4) 1.1549(2) 1.4549(4) 0.0835(13) Uani 1 1 d . . . F43 F 0.3113(5) 1.07821(19) 1.4517(3) 0.1047(18) Uani 1 1 d . . . F44 F 0.2574(4) 1.16102(17) 1.3254(3) 0.0651(10) Uani 1 1 d . . . F45 F 0.2989(4) 1.23759(18) 1.4630(3) 0.0691(10) Uani 1 1 d . . . F46 F 0.3491(4) 1.15388(18) 1.5873(3) 0.0721(12) Uani 1 1 d . . . C51 C 0.2250(7) 1.0863(4) 1.0764(6) 0.079(2) Uani 1 1 d . . . H51A H 0.2575 1.1082 1.1497 0.095 Uiso 1 1 calc R . . H51B H 0.2914 1.0855 1.0436 0.095 Uiso 1 1 calc R . . Cl52 Cl 0.1020(2) 1.13429(13) 0.99163(16) 0.0925(7) Uani 1 1 d . . . Cl53 Cl 0.1816(2) 1.00286(14) 1.09299(18) 0.0969(7) Uani 1 1 d . . . C61 C 0.2708(9) 0.8390(3) 1.3854(9) 0.097(3) Uani 1 1 d . . . H61A H 0.3525 0.8182 1.4003 0.117 Uiso 1 1 calc R . . H61B H 0.2336 0.8194 1.4380 0.117 Uiso 1 1 calc R . . Cl62 Cl 0.1825(2) 0.81998(16) 1.2559(3) 0.1334(12) Uani 1 1 d . . . Cl63 Cl 0.28801(18) 0.92577(10) 1.40739(15) 0.0746(5) 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 Ag 0.0489(3) 0.0117(2) 0.0531(3) -0.00296(15) 0.01132(19) 0.00025(15) N11 0.037(2) 0.0129(18) 0.040(2) -0.0030(15) 0.0090(17) 0.0015(15) C12 0.075(4) 0.019(3) 0.063(3) 0.003(2) 0.043(3) -0.003(2) C13 0.070(4) 0.020(2) 0.060(3) -0.004(2) 0.042(3) -0.002(2) C14 0.028(2) 0.015(2) 0.030(2) 0.0006(17) 0.0041(18) 0.0006(17) C15 0.042(3) 0.018(2) 0.029(2) -0.0026(18) 0.011(2) -0.0005(19) C16 0.039(3) 0.019(2) 0.035(2) -0.0038(19) 0.012(2) 0.0028(19) N17 0.037(2) 0.0122(17) 0.0274(19) -0.0013(14) 0.0109(16) 0.0004(15) C18 0.065(3) 0.018(2) 0.036(3) -0.0025(19) 0.017(2) 0.005(2) C19 0.035(3) 0.019(2) 0.040(3) 0.0002(19) 0.010(2) -0.0012(19) O20 0.085(3) 0.0195(18) 0.082(3) 0.0042(18) 0.064(3) 0.0024(18) C21 0.032(2) 0.013(2) 0.036(2) -0.0013(18) 0.0066(19) 0.0001(17) S22 0.0318(6) 0.0125(5) 0.0433(6) -0.0006(4) 0.0126(5) 0.0003(4) C23 0.030(2) 0.017(2) 0.031(2) -0.0021(17) 0.0060(18) 0.0029(18) C24 0.028(2) 0.017(2) 0.040(2) 0.0010(19) 0.0085(19) 0.0053(18) C25 0.029(2) 0.018(2) 0.041(3) 0.0017(19) 0.008(2) -0.0026(18) C26 0.037(3) 0.014(2) 0.037(3) 0.0009(18) 0.012(2) 0.0016(18) O27 0.079(3) 0.0190(17) 0.054(2) -0.0043(16) 0.040(2) -0.0015(17) N28 0.033(2) 0.0132(18) 0.036(2) 0.0011(15) 0.0104(17) 0.0000(14) C29 0.059(3) 0.023(2) 0.033(2) 0.001(2) 0.017(2) -0.003(2) C30 0.028(2) 0.014(2) 0.033(2) -0.0006(18) 0.0084(18) -0.0018(17) C31 0.062(3) 0.024(3) 0.049(3) -0.001(2) 0.034(3) 0.000(2) C32 0.059(3) 0.024(3) 0.055(3) -0.008(2) 0.032(3) 0.000(2) N33 0.034(2) 0.0117(19) 0.046(2) -0.0019(16) 0.0083(18) -0.0009(15) C34 0.044(3) 0.017(2) 0.050(3) -0.002(2) 0.023(2) 0.000(2) C35 0.040(3) 0.019(2) 0.043(3) -0.003(2) 0.022(2) 0.0007(19) P40 0.0406(7) 0.0287(7) 0.0321(7) 0.0011(5) 0.0132(5) 0.0072(5) F41 0.052(3) 0.200(7) 0.117(4) -0.029(4) 0.037(3) 0.002(3) F42 0.050(2) 0.114(4) 0.090(3) 0.009(2) 0.028(2) -0.007(2) F43 0.194(5) 0.031(2) 0.067(3) -0.0034(18) 0.015(3) 0.033(3) F44 0.100(3) 0.059(2) 0.0340(17) -0.0047(14) 0.0199(18) -0.0054(19) F45 0.104(3) 0.041(2) 0.055(2) -0.0017(16) 0.017(2) -0.0046(19) F46 0.106(3) 0.061(2) 0.0360(18) 0.0056(15) 0.0047(18) 0.021(2) C51 0.073(5) 0.112(7) 0.057(4) -0.005(4) 0.029(3) 0.031(5) Cl52 0.0920(14) 0.1285(18) 0.0665(11) 0.0145(12) 0.0390(10) 0.0496(13) Cl53 0.0945(14) 0.121(2) 0.0952(14) 0.0285(13) 0.0591(12) 0.0318(13) C61 0.127(7) 0.049(4) 0.164(9) -0.027(5) 0.114(7) -0.016(4) Cl62 0.0935(16) 0.158(3) 0.163(3) -0.106(2) 0.0622(17) -0.0602(17) Cl63 0.0865(12) 0.0735(12) 0.0682(10) -0.0126(9) 0.0314(9) -0.0133(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 Ag N11 2.131(4) . ? Ag N33 2.140(4) 1_545 ? N11 C16 1.334(6) . ? N11 C12 1.353(7) . ? C12 C13 1.356(7) . ? C12 H12A 0.9500 . ? C13 C14 1.405(7) . ? C13 H13A 0.9500 . ? C14 C15 1.385(7) . ? C14 N17 1.405(5) . ? C15 C16 1.371(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N17 C19 1.392(6) . ? N17 C18 1.470(6) . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? C19 O20 1.215(6) . ? C19 C21 1.485(6) . ? C21 C25 1.361(6) . ? C21 S22 1.728(5) . ? S22 C23 1.721(4) . ? C23 C24 1.370(6) . ? C23 C26 1.493(6) . ? C24 C25 1.408(6) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 O27 1.209(6) . ? C26 N28 1.382(6) . ? N28 C30 1.415(5) . ? N28 C29 1.473(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.381(6) . ? C30 C31 1.388(7) . ? C31 C32 1.361(7) . ? C31 H31A 0.9500 . ? C32 N33 1.341(7) . ? C32 H32A 0.9500 . ? N33 C34 1.334(6) . ? N33 Ag 2.139(4) 1_565 ? C34 C35 1.372(6) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? P40 F43 1.560(4) . ? P40 F41 1.561(5) . ? P40 F42 1.577(4) . ? P40 F44 1.578(3) . ? P40 F46 1.599(4) . ? P40 F45 1.601(4) . ? C51 Cl52 1.756(7) . ? C51 Cl53 1.759(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C61 Cl62 1.682(11) . ? C61 Cl63 1.740(7) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag N33 168.62(16) . 1_545 ? C16 N11 C12 115.3(4) . . ? C16 N11 Ag 124.5(3) . . ? C12 N11 Ag 120.1(3) . . ? N11 C12 C13 124.0(5) . . ? N11 C12 H12A 118.0 . . ? C13 C12 H12A 118.0 . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 115.4(4) . . ? C15 C14 N17 126.2(4) . . ? C13 C14 N17 118.4(4) . . ? C16 C15 C14 120.3(4) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? N11 C16 C15 124.5(4) . . ? N11 C16 H16A 117.8 . . ? C15 C16 H16A 117.8 . . ? C19 N17 C14 122.0(4) . . ? C19 N17 C18 120.5(4) . . ? C14 N17 C18 117.3(3) . . ? N17 C18 H18D 109.5 . . ? N17 C18 H18E 109.5 . . ? H18D C18 H18E 109.5 . . ? N17 C18 H18F 109.5 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? O20 C19 N17 123.6(4) . . ? O20 C19 C21 118.9(4) . . ? N17 C19 C21 117.5(4) . . ? C25 C21 C19 133.0(4) . . ? C25 C21 S22 111.0(3) . . ? C19 C21 S22 115.7(3) . . ? C23 S22 C21 91.6(2) . . ? C24 C23 C26 131.1(4) . . ? C24 C23 S22 111.3(3) . . ? C26 C23 S22 117.2(3) . . ? C23 C24 C25 112.6(4) . . ? C23 C24 H24A 123.7 . . ? C25 C24 H24A 123.7 . . ? C21 C25 C24 113.4(4) . . ? C21 C25 H25A 123.3 . . ? C24 C25 H25A 123.3 . . ? O27 C26 N28 124.4(4) . . ? O27 C26 C23 118.8(4) . . ? N28 C26 C23 116.8(4) . . ? C26 N28 C30 121.8(4) . . ? C26 N28 C29 121.1(4) . . ? C30 N28 C29 117.0(4) . . ? N28 C29 H29A 109.5 . . ? N28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 116.3(4) . . ? C35 C30 N28 124.9(4) . . ? C31 C30 N28 118.8(4) . . ? C32 C31 C30 120.3(5) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? N33 C32 C31 123.6(5) . . ? N33 C32 H32A 118.2 . . ? C31 C32 H32A 118.2 . . ? C34 N33 C32 116.3(4) . . ? C34 N33 Ag 123.9(3) . 1_565 ? C32 N33 Ag 119.8(3) . 1_565 ? N33 C34 C35 123.5(5) . . ? N33 C34 H34A 118.3 . . ? C35 C34 H34A 118.3 . . ? C34 C35 C30 120.1(4) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? F43 P40 F41 92.0(3) . . ? F43 P40 F42 92.1(3) . . ? F41 P40 F42 175.6(3) . . ? F43 P40 F44 91.2(2) . . ? F41 P40 F44 91.5(3) . . ? F42 P40 F44 90.1(2) . . ? F43 P40 F46 89.6(2) . . ? F41 P40 F46 89.7(3) . . ? F42 P40 F46 88.7(2) . . ? F44 P40 F46 178.5(2) . . ? F43 P40 F45 178.4(2) . . ? F41 P40 F45 87.9(3) . . ? F42 P40 F45 88.0(2) . . ? F44 P40 F45 90.35(18) . . ? F46 P40 F45 88.79(19) . . ? Cl52 C51 Cl53 112.1(4) . . ? Cl52 C51 H51A 109.2 . . ? Cl53 C51 H51A 109.2 . . ? Cl52 C51 H51B 109.2 . . ? Cl53 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? Cl62 C61 Cl63 112.4(6) . . ? Cl62 C61 H61A 109.1 . . ? Cl63 C61 H61A 109.1 . . ? Cl62 C61 H61B 109.1 . . ? Cl63 C61 H61B 109.1 . . ? H61A C61 H61B 107.9 . . ? 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 N33 Ag N11 C16 168.9(6) 1_545 . . . ? N33 Ag N11 C12 -14.2(9) 1_545 . . . ? C16 N11 C12 C13 -0.2(8) . . . . ? Ag N11 C12 C13 -177.3(5) . . . . ? N11 C12 C13 C14 0.9(9) . . . . ? C12 C13 C14 C15 -1.4(8) . . . . ? C12 C13 C14 N17 180.0(5) . . . . ? C13 C14 C15 C16 1.3(6) . . . . ? N17 C14 C15 C16 179.7(4) . . . . ? C12 N11 C16 C15 0.0(7) . . . . ? Ag N11 C16 C15 177.0(3) . . . . ? C14 C15 C16 N11 -0.6(7) . . . . ? C15 C14 N17 C19 4.9(7) . . . . ? C13 C14 N17 C19 -176.7(4) . . . . ? C15 C14 N17 C18 -169.1(4) . . . . ? C13 C14 N17 C18 9.4(6) . . . . ? C14 N17 C19 O20 -11.7(7) . . . . ? C18 N17 C19 O20 162.1(5) . . . . ? C14 N17 C19 C21 168.5(4) . . . . ? C18 N17 C19 C21 -17.7(6) . . . . ? O20 C19 C21 C25 142.6(5) . . . . ? N17 C19 C21 C25 -37.7(7) . . . . ? O20 C19 C21 S22 -30.7(6) . . . . ? N17 C19 C21 S22 149.0(3) . . . . ? C25 C21 S22 C23 3.4(4) . . . . ? C19 C21 S22 C23 178.1(3) . . . . ? C21 S22 C23 C24 -2.9(4) . . . . ? C21 S22 C23 C26 -176.1(3) . . . . ? C26 C23 C24 C25 173.7(4) . . . . ? S22 C23 C24 C25 1.8(5) . . . . ? C19 C21 C25 C24 -176.5(5) . . . . ? S22 C21 C25 C24 -3.0(5) . . . . ? C23 C24 C25 C21 0.8(6) . . . . ? C24 C23 C26 O27 -130.4(5) . . . . ? S22 C23 C26 O27 41.1(6) . . . . ? C24 C23 C26 N28 48.0(7) . . . . ? S22 C23 C26 N28 -140.5(3) . . . . ? O27 C26 N28 C30 13.0(7) . . . . ? C23 C26 N28 C30 -165.2(4) . . . . ? O27 C26 N28 C29 -170.2(5) . . . . ? C23 C26 N28 C29 11.5(6) . . . . ? C26 N28 C30 C35 -22.3(7) . . . . ? C29 N28 C30 C35 160.8(4) . . . . ? C26 N28 C30 C31 158.8(4) . . . . ? C29 N28 C30 C31 -18.1(6) . . . . ? C35 C30 C31 C32 -0.7(8) . . . . ? N28 C30 C31 C32 178.3(5) . . . . ? C30 C31 C32 N33 0.6(9) . . . . ? C31 C32 N33 C34 -0.2(8) . . . . ? C31 C32 N33 Ag -176.7(4) . . . 1_565 ? C32 N33 C34 C35 -0.1(7) . . . . ? Ag N33 C34 C35 176.2(4) 1_565 . . . ? N33 C34 C35 C30 0.0(8) . . . . ? C31 C30 C35 C34 0.4(7) . . . . ? N28 C30 C35 C34 -178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.387 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.101 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 604514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 N4 O2 S' _chemical_formula_weight 352.41 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.0773(8) _cell_length_b 7.3465(10) _cell_length_c 9.7829(16) _cell_angle_alpha 102.253(8) _cell_angle_beta 91.961(9) _cell_angle_gamma 109.728(8) _cell_volume 399.10(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 852 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description petal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 184 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8637 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3205 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1870 _reflns_number_gt 1761 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0265P)^2^+0.4921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.19(13) _refine_ls_number_reflns 1870 _refine_ls_number_parameters 226 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.134 _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 N11 N 1.0726(7) 0.8371(6) 0.8753(5) 0.0338(10) Uani 1 1 d . . . C12 C 0.8970(9) 0.8019(7) 0.7744(5) 0.0305(12) Uani 1 1 d . . . H12A H 0.9384 0.8186 0.6839 0.037 Uiso 1 1 calc R . . C13 C 0.6626(8) 0.7438(6) 0.7928(5) 0.0257(11) Uani 1 1 d . . . C14 C 0.6045(8) 0.7195(7) 0.9266(5) 0.0302(11) Uani 1 1 d . . . H14A H 0.4449 0.6829 0.9451 0.036 Uiso 1 1 calc R . . C15 C 0.7771(8) 0.7486(7) 1.0303(5) 0.0303(11) Uani 1 1 d . . . H15A H 0.7396 0.7292 1.1209 0.036 Uiso 1 1 calc R . . C16 C 1.0098(9) 0.8074(7) 1.0002(6) 0.0323(12) Uani 1 1 d . . . H16A H 1.1298 0.8272 1.0725 0.039 Uiso 1 1 calc R . . C17 C 0.4793(8) 0.7070(6) 0.6747(5) 0.0271(11) Uani 1 1 d . . . H17A H 0.3669 0.7723 0.7092 0.033 Uiso 1 1 calc R . . H17B H 0.5553 0.7679 0.5994 0.033 Uiso 1 1 calc R . . N18 N 0.3497(6) 0.4936(5) 0.6156(4) 0.0261(9) Uani 1 1 d . . . H18A H 0.2151 0.4347 0.6456 0.031 Uiso 1 1 calc R . . C19 C 0.4339(8) 0.3892(7) 0.5175(5) 0.0247(11) Uani 1 1 d . . . O20 O 0.6199(5) 0.4590(5) 0.4679(4) 0.0321(9) Uani 1 1 d . . . C21 C 0.2909(8) 0.1724(7) 0.4674(5) 0.0266(11) Uani 1 1 d . . . S22 S 0.42539(17) 0.01662(15) 0.38199(13) 0.0295(3) Uani 1 1 d . . . C23 C 0.1695(8) -0.1868(7) 0.3618(5) 0.0272(11) Uani 1 1 d . . . C24 C -0.0115(8) -0.1338(7) 0.4137(5) 0.0272(11) Uani 1 1 d . . . H24A H -0.1675 -0.2247 0.4086 0.033 Uiso 1 1 calc R . . C25 C 0.0603(8) 0.0720(7) 0.4757(5) 0.0274(11) Uani 1 1 d . . . H25A H -0.0420 0.1342 0.5190 0.033 Uiso 1 1 calc R . . C26 C 0.1753(9) -0.3795(7) 0.2814(5) 0.0269(11) Uani 1 1 d . . . O27 O 0.3494(6) -0.3864(5) 0.2213(4) 0.0377(9) Uani 1 1 d . . . N28 N -0.0152(7) -0.5409(5) 0.2761(4) 0.0304(10) Uani 1 1 d . . . H28A H -0.1260 -0.5321 0.3300 0.036 Uiso 1 1 calc R . . C29 C -0.0410(9) -0.7331(7) 0.1808(5) 0.0314(11) Uani 1 1 d . . . H29A H -0.1586 -0.8420 0.2123 0.038 Uiso 1 1 calc R . . H29B H 0.1112 -0.7546 0.1848 0.038 Uiso 1 1 calc R . . C30 C -0.1177(8) -0.7390(7) 0.0313(5) 0.0241(10) Uani 1 1 d . . . C31 C 0.0477(8) -0.6840(6) -0.0617(5) 0.0278(11) Uani 1 1 d . . . H31A H 0.2087 -0.6502 -0.0289 0.033 Uiso 1 1 calc R . . N32 N -0.0033(7) -0.6756(6) -0.1926(4) 0.0290(9) Uani 1 1 d . . . C33 C -0.2290(9) -0.7220(7) -0.2359(6) 0.0307(12) Uani 1 1 d . . . H33A H -0.2693 -0.7127 -0.3282 0.037 Uiso 1 1 calc R . . C34 C -0.4071(8) -0.7823(7) -0.1554(5) 0.0307(12) Uani 1 1 d . . . H34A H -0.5664 -0.8170 -0.1921 0.037 Uiso 1 1 calc R . . C35 C -0.3503(8) -0.7920(7) -0.0188(5) 0.0303(11) Uani 1 1 d . . . H35A H -0.4707 -0.8347 0.0391 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N11 0.026(2) 0.039(2) 0.035(2) 0.009(2) 0.0033(19) 0.0091(19) C12 0.026(2) 0.035(3) 0.030(3) 0.006(2) 0.005(2) 0.010(2) C13 0.029(3) 0.016(2) 0.031(3) 0.002(2) 0.000(2) 0.008(2) C14 0.024(2) 0.028(2) 0.034(3) 0.000(2) 0.006(2) 0.009(2) C15 0.035(3) 0.028(2) 0.029(3) 0.009(2) 0.007(2) 0.011(2) C16 0.031(3) 0.034(3) 0.029(3) 0.003(2) 0.000(2) 0.012(2) C17 0.029(3) 0.020(2) 0.031(3) 0.002(2) 0.004(2) 0.009(2) N18 0.018(2) 0.026(2) 0.029(2) 0.0019(18) 0.0019(16) 0.0046(16) C19 0.019(2) 0.026(2) 0.028(3) 0.008(2) 0.001(2) 0.006(2) O20 0.0272(19) 0.0285(18) 0.036(2) 0.0049(16) 0.0078(16) 0.0049(16) C21 0.025(2) 0.027(2) 0.024(3) 0.003(2) 0.002(2) 0.007(2) S22 0.0224(6) 0.0284(6) 0.0342(7) 0.0036(5) 0.0060(5) 0.0065(5) C23 0.030(3) 0.024(2) 0.026(3) 0.007(2) 0.002(2) 0.007(2) C24 0.021(2) 0.029(2) 0.027(3) 0.007(2) 0.0063(19) 0.003(2) C25 0.029(3) 0.027(2) 0.026(3) 0.005(2) 0.008(2) 0.010(2) C26 0.032(3) 0.028(3) 0.024(3) 0.008(2) 0.006(2) 0.013(2) O27 0.032(2) 0.035(2) 0.043(2) 0.0006(17) 0.0108(17) 0.0124(17) N28 0.037(2) 0.026(2) 0.026(2) 0.0029(18) 0.0119(19) 0.0092(19) C29 0.037(3) 0.026(2) 0.030(3) 0.005(2) 0.007(2) 0.010(2) C30 0.027(2) 0.021(2) 0.025(3) 0.005(2) 0.002(2) 0.0096(19) C31 0.033(3) 0.023(2) 0.024(3) -0.001(2) 0.008(2) 0.008(2) N32 0.028(2) 0.028(2) 0.030(2) 0.0047(18) 0.0050(18) 0.0091(18) C33 0.034(3) 0.030(3) 0.027(3) 0.001(2) 0.000(2) 0.014(2) C34 0.022(2) 0.031(2) 0.042(3) 0.007(2) 0.001(2) 0.015(2) C35 0.029(3) 0.029(3) 0.033(3) 0.006(2) 0.011(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C16 1.333(7) . ? N11 C12 1.346(6) . ? C12 C13 1.372(7) . ? C12 H12A 0.9500 . ? C13 C14 1.399(7) . ? C13 C17 1.491(6) . ? C14 C15 1.364(7) . ? C14 H14A 0.9500 . ? C15 C16 1.394(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 N18 1.471(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N18 C19 1.326(6) . ? N18 H18A 0.8800 . ? C19 O20 1.236(6) . ? C19 C21 1.496(6) . ? C21 C25 1.360(6) . ? C21 S22 1.717(5) . ? S22 C23 1.725(4) . ? C23 C24 1.364(7) . ? C23 C26 1.479(7) . ? C24 C25 1.411(6) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 O27 1.238(6) . ? C26 N28 1.339(6) . ? N28 C29 1.473(6) . ? N28 H28A 0.8800 . ? C29 C30 1.507(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C35 1.375(6) . ? C30 C31 1.395(6) . ? C31 N32 1.327(6) . ? C31 H31A 0.9500 . ? N32 C33 1.327(6) . ? C33 C34 1.367(7) . ? C33 H33A 0.9500 . ? C34 C35 1.392(7) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? 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 C16 N11 C12 116.5(4) . . ? N11 C12 C13 124.8(5) . . ? N11 C12 H12A 117.6 . . ? C13 C12 H12A 117.6 . . ? C12 C13 C14 116.9(4) . . ? C12 C13 C17 121.2(4) . . ? C14 C13 C17 121.9(4) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 118.4(5) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? N11 C16 C15 123.4(5) . . ? N11 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? N18 C17 C13 112.4(4) . . ? N18 C17 H17A 109.1 . . ? C13 C17 H17A 109.1 . . ? N18 C17 H17B 109.1 . . ? C13 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C19 N18 C17 120.6(4) . . ? C19 N18 H18A 119.7 . . ? C17 N18 H18A 119.7 . . ? O20 C19 N18 124.4(4) . . ? O20 C19 C21 119.5(4) . . ? N18 C19 C21 116.1(4) . . ? C25 C21 C19 130.2(4) . . ? C25 C21 S22 111.6(3) . . ? C19 C21 S22 118.2(3) . . ? C21 S22 C23 91.2(2) . . ? C24 C23 C26 131.3(4) . . ? C24 C23 S22 111.8(4) . . ? C26 C23 S22 116.5(4) . . ? C23 C24 C25 112.0(4) . . ? C23 C24 H24A 124.0 . . ? C25 C24 H24A 124.0 . . ? C21 C25 C24 113.2(4) . . ? C21 C25 H25A 123.4 . . ? C24 C25 H25A 123.4 . . ? O27 C26 N28 122.9(5) . . ? O27 C26 C23 120.2(4) . . ? N28 C26 C23 116.8(4) . . ? C26 N28 C29 120.5(4) . . ? C26 N28 H28A 119.7 . . ? C29 N28 H28A 119.7 . . ? N28 C29 C30 111.2(4) . . ? N28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? N28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C35 C30 C31 116.9(4) . . ? C35 C30 C29 122.3(4) . . ? C31 C30 C29 120.7(4) . . ? N32 C31 C30 124.8(5) . . ? N32 C31 H31A 117.6 . . ? C30 C31 H31A 117.6 . . ? C31 N32 C33 116.6(4) . . ? N32 C33 C34 123.8(5) . . ? N32 C33 H33A 118.1 . . ? C34 C33 H33A 118.1 . . ? C33 C34 C35 118.7(5) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C30 C35 C34 119.1(4) . . ? C30 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? 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 C16 N11 C12 C13 1.8(8) . . . . ? N11 C12 C13 C14 -0.1(8) . . . . ? N11 C12 C13 C17 -179.7(4) . . . . ? C12 C13 C14 C15 -1.7(7) . . . . ? C17 C13 C14 C15 177.9(5) . . . . ? C13 C14 C15 C16 1.7(7) . . . . ? C12 N11 C16 C15 -1.8(7) . . . . ? C14 C15 C16 N11 0.2(8) . . . . ? C12 C13 C17 N18 104.7(5) . . . . ? C14 C13 C17 N18 -74.9(5) . . . . ? C13 C17 N18 C19 -84.9(5) . . . . ? C17 N18 C19 O20 -0.6(7) . . . . ? C17 N18 C19 C21 178.5(4) . . . . ? O20 C19 C21 C25 -160.7(5) . . . . ? N18 C19 C21 C25 20.1(7) . . . . ? O20 C19 C21 S22 17.9(6) . . . . ? N18 C19 C21 S22 -161.3(3) . . . . ? C25 C21 S22 C23 -1.5(4) . . . . ? C19 C21 S22 C23 179.6(4) . . . . ? C21 S22 C23 C24 2.4(4) . . . . ? C21 S22 C23 C26 176.5(4) . . . . ? C26 C23 C24 C25 -175.6(5) . . . . ? S22 C23 C24 C25 -2.6(5) . . . . ? C19 C21 C25 C24 179.1(5) . . . . ? S22 C21 C25 C24 0.4(5) . . . . ? C23 C24 C25 C21 1.5(6) . . . . ? C24 C23 C26 O27 166.0(5) . . . . ? S22 C23 C26 O27 -6.8(6) . . . . ? C24 C23 C26 N28 -13.1(7) . . . . ? S22 C23 C26 N28 174.2(4) . . . . ? O27 C26 N28 C29 -8.7(7) . . . . ? C23 C26 N28 C29 170.3(4) . . . . ? C26 N28 C29 C30 -78.1(6) . . . . ? N28 C29 C30 C35 -85.4(5) . . . . ? N28 C29 C30 C31 92.6(5) . . . . ? C35 C30 C31 N32 1.5(7) . . . . ? C29 C30 C31 N32 -176.6(4) . . . . ? C30 C31 N32 C33 0.5(7) . . . . ? C31 N32 C33 C34 -2.1(7) . . . . ? N32 C33 C34 C35 1.5(7) . . . . ? C31 C30 C35 C34 -2.0(7) . . . . ? C29 C30 C35 C34 176.1(4) . . . . ? C33 C34 C35 C30 0.6(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N18 H18A N32 0.88 2.21 3.022(6) 153.3 1_566 N28 H28A O20 0.88 2.08 2.953(5) 172.4 1_445 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.280 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.055 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 604515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21.50 H19 Ag F3 N4 O4.50 S' _chemical_formula_weight 602.34 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7057(11) _cell_length_b 12.7485(16) _cell_length_c 14.185(2) _cell_angle_alpha 112.983(7) _cell_angle_beta 104.112(6) _cell_angle_gamma 94.866(8) _cell_volume 1218.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7929 _exptl_absorpt_correction_T_max 0.9761 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _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 6017 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4178 _reflns_number_gt 2610 _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^)+(0.1175P)^2^+7.1321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 4178 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2475 _refine_ls_wR_factor_gt 0.2135 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.355 _refine_ls_shift/su_mean 0.016 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 Ag Ag 1.60928(12) 0.98638(8) 0.91577(7) 0.0548(4) Uani 1 1 d . . . N11 N 1.4412(12) 1.0225(7) 0.7886(7) 0.045(2) Uani 1 1 d . . . C12 C 1.4169(14) 1.1323(9) 0.8092(8) 0.044(2) Uani 1 1 d . . . H12A H 1.4750 1.1913 0.8796 0.052 Uiso 1 1 calc R . . C13 C 1.3139(14) 1.1639(9) 0.7349(8) 0.044(2) Uani 1 1 d . . . C14 C 1.2280(16) 1.0801(10) 0.6346(9) 0.055(3) Uani 1 1 d . . . H14A H 1.1540 1.0985 0.5813 0.066 Uiso 1 1 calc R . . C15 C 1.2508(19) 0.9658(10) 0.6115(10) 0.070(4) Uani 1 1 d . . . H15A H 1.1922 0.9053 0.5418 0.084 Uiso 1 1 calc R . . C16 C 1.3558(16) 0.9421(11) 0.6880(9) 0.061(3) Uani 1 1 d . . . H16A H 1.3708 0.8642 0.6702 0.074 Uiso 1 1 calc R . . C17 C 1.2990(17) 1.2900(9) 0.7714(9) 0.053(3) Uani 1 1 d . . . H17A H 1.2781 1.3180 0.8426 0.064 Uiso 1 1 calc R . . H17B H 1.4165 1.3362 0.7800 0.064 Uiso 1 1 calc R . . N18 N 1.1514(11) 1.3105(7) 0.6968(7) 0.045(2) Uani 1 1 d . . . H18A H 1.1752 1.3273 0.6461 0.054 Uiso 1 1 calc R . . C19 C 0.9830(14) 1.3044(8) 0.7044(8) 0.040(2) Uani 1 1 d . . . O20 O 0.9391(11) 1.2783(7) 0.7719(6) 0.058(2) Uani 1 1 d . . . C21 C 0.8456(15) 1.3278(9) 0.6264(8) 0.045(2) Uani 1 1 d . . . S22 S 0.6210(4) 1.2902(3) 0.6155(2) 0.0511(7) Uani 1 1 d . . . C23 C 0.5518(14) 1.3358(9) 0.5150(9) 0.049(3) Uani 1 1 d . . . C24 C 0.6930(15) 1.3778(10) 0.4919(9) 0.054(3) Uani 1 1 d . . . H24A H 0.6804 1.4066 0.4385 0.065 Uiso 1 1 calc R . . C25 C 0.8640(14) 1.3746(9) 0.5562(9) 0.048(3) Uani 1 1 d . . . H25A H 0.9785 1.4017 0.5511 0.058 Uiso 1 1 calc R . . C26 C 0.3544(17) 1.3192(11) 0.4651(10) 0.063(3) Uani 1 1 d . . . O27 O 0.2436(11) 1.3083(9) 0.5132(7) 0.078(3) Uani 1 1 d . . . N28 N 0.3028(13) 1.3104(9) 0.3663(8) 0.062(3) Uani 1 1 d . . . H28A H 0.3878 1.3197 0.3370 0.075 Uiso 1 1 calc R . . C29 C 0.1105(16) 1.2857(13) 0.3027(10) 0.069(4) Uani 1 1 d . . . H29A H 0.0964 1.3334 0.2615 0.083 Uiso 1 1 calc R . . H29B H 0.0346 1.3081 0.3517 0.083 Uiso 1 1 calc R . . C30 C 0.0435(15) 1.1593(11) 0.2261(10) 0.056(3) Uani 1 1 d . . . C31 C -0.0916(14) 1.1298(10) 0.1321(9) 0.050(3) Uani 1 1 d . . . H31A H -0.1338 1.1899 0.1149 0.060 Uiso 1 1 calc R . . N32 N -0.1660(11) 1.0190(7) 0.0638(7) 0.044(2) Uani 1 1 d . . . C33 C -0.1071(14) 0.9349(11) 0.0830(11) 0.059(3) Uani 1 1 d . . . H33A H -0.1597 0.8567 0.0327 0.071 Uiso 1 1 calc R . . C34 C 0.0283(16) 0.9566(12) 0.1736(12) 0.065(4) Uani 1 1 d . . . H34A H 0.0694 0.8937 0.1862 0.078 Uiso 1 1 calc R . . C35 C 0.1063(17) 1.0688(13) 0.2471(11) 0.068(4) Uani 1 1 d . . . H35A H 0.2008 1.0846 0.3110 0.081 Uiso 1 1 calc R . . O41 O 0.4880(12) 1.2379(7) 0.2146(7) 0.063(2) Uani 1 1 d . . . O42 O 0.5299(11) 1.2084(7) 0.0582(6) 0.059(2) Uani 1 1 d . . . C43 C 0.5197(16) 1.2690(9) 0.1478(9) 0.052(3) Uani 1 1 d . . . C44 C 0.564(6) 1.3945(15) 0.1820(17) 0.192(17) Uani 1 1 d . . . F45 F 0.791(2) 1.4205(12) 0.2355(18) 0.218(10) Uani 1 1 d . . . F46 F 0.547(2) 1.4333(8) 0.1097(9) 0.169(6) Uani 1 1 d . . . F47 F 0.5470(18) 1.4651(7) 0.2616(9) 0.119(4) Uani 1 1 d . . . C51 C -0.146(6) 1.410(3) 0.015(3) 0.112(12) Uani 0.50 1 d P A -1 H51A H -0.2243 1.3466 0.0173 0.168 Uiso 0.50 1 calc PR A -1 H51B H -0.1784 1.4040 -0.0582 0.168 Uiso 0.50 1 calc PR A -1 H51C H -0.1644 1.4848 0.0637 0.168 Uiso 0.50 1 calc PR A -1 C52 C 0.072(5) 1.401(4) 0.054(3) 0.15(2) Uani 0.50 1 d P A -1 C53 C 0.176(4) 1.511(2) 0.040(3) 0.092(10) Uani 0.50 1 d P A -1 H53A H 0.3082 1.5157 0.0602 0.138 Uiso 0.50 1 calc PR A -1 H53B H 0.1485 1.5842 0.0859 0.138 Uiso 0.50 1 calc PR A -1 H53C H 0.1319 1.4994 -0.0354 0.138 Uiso 0.50 1 calc PR A -1 O54 O 0.225(10) 1.380(4) 0.135(6) 0.37(5) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0548(6) 0.0535(6) 0.0524(6) 0.0279(4) 0.0016(4) 0.0080(4) N11 0.051(5) 0.036(5) 0.045(5) 0.015(4) 0.009(4) 0.013(4) C12 0.044(6) 0.053(6) 0.032(6) 0.019(5) 0.009(5) 0.006(5) C13 0.040(6) 0.047(6) 0.036(6) 0.013(5) 0.006(5) 0.005(5) C14 0.070(8) 0.054(7) 0.035(6) 0.019(5) 0.001(5) 0.023(6) C15 0.100(10) 0.050(7) 0.039(7) 0.006(5) 0.002(7) 0.033(7) C16 0.061(8) 0.056(7) 0.047(7) 0.009(6) 0.002(6) 0.015(6) C17 0.070(8) 0.040(6) 0.045(7) 0.017(5) 0.012(6) 0.015(5) N18 0.042(5) 0.051(5) 0.040(5) 0.021(4) 0.005(4) 0.014(4) C19 0.046(6) 0.038(5) 0.032(6) 0.016(4) 0.004(5) 0.004(4) O20 0.063(5) 0.068(5) 0.054(5) 0.037(4) 0.015(4) 0.010(4) C21 0.059(7) 0.041(6) 0.032(6) 0.009(5) 0.016(5) 0.012(5) S22 0.0462(16) 0.0645(18) 0.0422(16) 0.0217(14) 0.0142(13) 0.0116(13) C23 0.042(6) 0.052(6) 0.049(7) 0.019(5) 0.012(5) 0.008(5) C24 0.052(7) 0.054(7) 0.055(7) 0.024(6) 0.012(6) 0.017(6) C25 0.039(6) 0.056(7) 0.057(7) 0.031(6) 0.016(5) 0.011(5) C26 0.056(8) 0.073(8) 0.051(8) 0.016(6) 0.013(6) 0.030(7) O27 0.041(5) 0.130(8) 0.053(5) 0.024(5) 0.020(4) 0.022(5) N28 0.049(6) 0.089(7) 0.037(6) 0.021(5) 0.003(4) 0.017(5) C29 0.047(7) 0.100(10) 0.056(8) 0.028(8) 0.011(6) 0.030(7) C30 0.046(7) 0.086(9) 0.053(7) 0.040(7) 0.022(6) 0.023(6) C31 0.043(6) 0.061(7) 0.051(7) 0.028(6) 0.014(5) 0.008(5) N32 0.045(5) 0.033(4) 0.047(5) 0.019(4) 0.002(4) -0.001(4) C33 0.027(6) 0.078(8) 0.092(10) 0.060(8) 0.012(6) 0.010(5) C34 0.040(7) 0.075(9) 0.098(11) 0.059(9) 0.013(7) 0.011(6) C35 0.050(7) 0.103(11) 0.058(8) 0.045(8) 0.012(6) 0.015(7) O41 0.088(6) 0.063(5) 0.058(5) 0.034(4) 0.035(5) 0.031(5) O42 0.062(5) 0.062(5) 0.047(5) 0.021(4) 0.010(4) 0.005(4) C43 0.067(8) 0.046(6) 0.036(7) 0.015(5) 0.009(5) 0.006(5) C44 0.47(6) 0.040(9) 0.074(13) 0.026(9) 0.09(2) 0.049(18) F45 0.173(14) 0.111(10) 0.29(2) 0.085(12) -0.046(15) -0.012(10) F46 0.35(2) 0.062(6) 0.112(9) 0.052(6) 0.079(11) 0.028(8) F47 0.194(12) 0.051(5) 0.105(8) 0.022(5) 0.050(7) 0.026(6) C51 0.17(4) 0.07(2) 0.08(2) 0.016(18) 0.03(2) 0.03(2) C52 0.10(3) 0.16(4) 0.07(2) -0.08(2) 0.07(2) -0.08(3) C53 0.08(2) 0.067(18) 0.09(2) 0.000(16) 0.033(18) -0.006(16) O54 0.64(11) 0.18(3) 0.71(12) 0.34(6) 0.61(11) 0.30(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N11 2.180(8) . ? Ag N32 2.237(8) 1_756 ? Ag Ag 3.1752(19) 2_877 ? N11 C16 1.343(14) . ? N11 C12 1.354(12) . ? C12 C13 1.371(14) . ? C12 H12A 0.9500 . ? C13 C14 1.356(15) . ? C13 C17 1.508(14) . ? C14 C15 1.400(15) . ? C14 H14A 0.9500 . ? C15 C16 1.339(16) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 N18 1.470(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N18 C19 1.326(13) . ? N18 H18A 0.8800 . ? C19 O20 1.237(12) . ? C19 C21 1.475(14) . ? C21 C25 1.373(14) . ? C21 S22 1.708(11) . ? S22 C23 1.727(11) . ? C23 C24 1.339(15) . ? C23 C26 1.470(16) . ? C24 C25 1.422(15) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 O27 1.246(15) . ? C26 N28 1.317(15) . ? N28 C29 1.469(15) . ? N28 H28A 0.8800 . ? C29 C30 1.504(18) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.367(16) . ? C30 C35 1.395(17) . ? C31 N32 1.337(13) . ? C31 H31A 0.9500 . ? N32 C33 1.297(13) . ? N32 Ag 2.237(8) 1_354 ? C33 C34 1.355(17) . ? C33 H33A 0.9500 . ? C34 C35 1.371(19) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? O41 C43 1.228(13) . ? O42 C43 1.229(13) . ? C43 C44 1.46(2) . ? C44 F47 1.19(2) . ? C44 F46 1.287(19) . ? C44 F45 1.67(4) . ? C51 C52 1.67(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O54 1.55(8) . ? C52 C53 1.67(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? 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 Ag N32 158.0(3) . 1_756 ? N11 Ag Ag 107.1(2) . 2_877 ? N32 Ag Ag 78.3(2) 1_756 2_877 ? C16 N11 C12 115.6(9) . . ? C16 N11 Ag 124.6(7) . . ? C12 N11 Ag 119.8(7) . . ? N11 C12 C13 124.3(10) . . ? N11 C12 H12A 117.9 . . ? C13 C12 H12A 117.9 . . ? C14 C13 C12 118.3(10) . . ? C14 C13 C17 124.1(9) . . ? C12 C13 C17 117.6(9) . . ? C13 C14 C15 118.4(10) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 119.6(11) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? N11 C16 C15 123.7(11) . . ? N11 C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? N18 C17 C13 113.6(9) . . ? N18 C17 H17A 108.9 . . ? C13 C17 H17A 108.9 . . ? N18 C17 H17B 108.9 . . ? C13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 N18 C17 121.4(9) . . ? C19 N18 H18A 119.3 . . ? C17 N18 H18A 119.3 . . ? O20 C19 N18 122.6(9) . . ? O20 C19 C21 120.3(9) . . ? N18 C19 C21 117.1(9) . . ? C25 C21 C19 131.2(10) . . ? C25 C21 S22 111.2(8) . . ? C19 C21 S22 117.6(8) . . ? C21 S22 C23 91.5(5) . . ? C24 C23 C26 129.8(11) . . ? C24 C23 S22 112.3(8) . . ? C26 C23 S22 117.8(9) . . ? C23 C24 C25 112.3(10) . . ? C23 C24 H24A 123.8 . . ? C25 C24 H24A 123.8 . . ? C21 C25 C24 112.7(10) . . ? C21 C25 H25A 123.7 . . ? C24 C25 H25A 123.7 . . ? O27 C26 N28 122.7(11) . . ? O27 C26 C23 120.7(11) . . ? N28 C26 C23 116.5(11) . . ? C26 N28 C29 123.2(11) . . ? C26 N28 H28A 118.4 . . ? C29 N28 H28A 118.4 . . ? N28 C29 C30 112.0(10) . . ? N28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? N28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C35 117.4(12) . . ? C31 C30 C29 118.8(10) . . ? C35 C30 C29 123.7(12) . . ? N32 C31 C30 121.9(11) . . ? N32 C31 H31A 119.0 . . ? C30 C31 H31A 119.0 . . ? C33 N32 C31 120.6(10) . . ? C33 N32 Ag 122.1(8) . 1_354 ? C31 N32 Ag 117.3(7) . 1_354 ? N32 C33 C34 121.1(13) . . ? N32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C33 C34 C35 120.4(12) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? C34 C35 C30 118.5(12) . . ? C34 C35 H35A 120.8 . . ? C30 C35 H35A 120.8 . . ? O42 C43 O41 128.3(11) . . ? O42 C43 C44 115.7(13) . . ? O41 C43 C44 115.9(12) . . ? F47 C44 F46 110.5(17) . . ? F47 C44 C43 124.5(19) . . ? F46 C44 C43 118.6(16) . . ? F47 C44 F45 92(2) . . ? F46 C44 F45 103(2) . . ? C43 C44 F45 100.5(19) . . ? C52 C51 H51A 109.0 . . ? C52 C51 H51B 109.8 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.7 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O54 C52 C53 104(3) . . ? O54 C52 C51 147(3) . . ? C53 C52 C51 101(4) . . ? C52 C53 H53A 109.0 . . ? C52 C53 H53B 109.7 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.7 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 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 N32 Ag N11 C16 149.0(9) 1_756 . . . ? Ag Ag N11 C16 -109.6(9) 2_877 . . . ? N32 Ag N11 C12 -31.3(13) 1_756 . . . ? Ag Ag N11 C12 70.1(8) 2_877 . . . ? C16 N11 C12 C13 -0.2(15) . . . . ? Ag N11 C12 C13 -179.9(8) . . . . ? N11 C12 C13 C14 1.0(16) . . . . ? N11 C12 C13 C17 179.3(9) . . . . ? C12 C13 C14 C15 -0.9(17) . . . . ? C17 C13 C14 C15 -179.0(11) . . . . ? C13 C14 C15 C16 0(2) . . . . ? C12 N11 C16 C15 -0.8(18) . . . . ? Ag N11 C16 C15 178.9(10) . . . . ? C14 C15 C16 N11 1(2) . . . . ? C14 C13 C17 N18 13.0(16) . . . . ? C12 C13 C17 N18 -165.2(9) . . . . ? C13 C17 N18 C19 88.3(12) . . . . ? C17 N18 C19 O20 -1.9(15) . . . . ? C17 N18 C19 C21 179.3(9) . . . . ? O20 C19 C21 C25 168.7(11) . . . . ? N18 C19 C21 C25 -12.5(16) . . . . ? O20 C19 C21 S22 -12.6(13) . . . . ? N18 C19 C21 S22 166.2(7) . . . . ? C25 C21 S22 C23 0.7(8) . . . . ? C19 C21 S22 C23 -178.2(8) . . . . ? C21 S22 C23 C24 -0.3(9) . . . . ? C21 S22 C23 C26 177.1(9) . . . . ? C26 C23 C24 C25 -177.2(11) . . . . ? S22 C23 C24 C25 -0.2(12) . . . . ? C19 C21 C25 C24 177.8(10) . . . . ? S22 C21 C25 C24 -1.0(12) . . . . ? C23 C24 C25 C21 0.7(14) . . . . ? C24 C23 C26 O27 -160.9(13) . . . . ? S22 C23 C26 O27 22.2(16) . . . . ? C24 C23 C26 N28 22.6(19) . . . . ? S22 C23 C26 N28 -154.3(10) . . . . ? O27 C26 N28 C29 -1(2) . . . . ? C23 C26 N28 C29 175.7(11) . . . . ? C26 N28 C29 C30 -98.6(14) . . . . ? N28 C29 C30 C31 -150.6(11) . . . . ? N28 C29 C30 C35 32.1(16) . . . . ? C35 C30 C31 N32 2.0(16) . . . . ? C29 C30 C31 N32 -175.4(10) . . . . ? C30 C31 N32 C33 -2.5(16) . . . . ? C30 C31 N32 Ag 178.4(8) . . . 1_354 ? C31 N32 C33 C34 1.4(17) . . . . ? Ag N32 C33 C34 -179.5(8) 1_354 . . . ? N32 C33 C34 C35 -0.1(19) . . . . ? C33 C34 C35 C30 -0.3(18) . . . . ? C31 C30 C35 C34 -0.6(17) . . . . ? C29 C30 C35 C34 176.7(11) . . . . ? O42 C43 C44 F47 173(3) . . . . ? O41 C43 C44 F47 -11(4) . . . . ? O42 C43 C44 F46 24(4) . . . . ? O41 C43 C44 F46 -160(2) . . . . ? O42 C43 C44 F45 -86.4(16) . . . . ? O41 C43 C44 F45 89(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.744 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.159 #===END