# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_w6 #TrackingRef '7-Ligand.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H8 N2 O' _chemical_formula_weight 220.22 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9698(17) _cell_length_b 9.389(2) _cell_length_c 15.464(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.310(5) _cell_angle_gamma 90.00 _cell_volume 1156.3(4) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9813 _exptl_absorpt_correction_T_max 0.9984 _exptl_absorpt_process_details 'blessing, Acta Cryst. 1995(A51) 33-38' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12578 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.65 _reflns_number_total 2181 _reflns_number_gt 1530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.1061P] 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 2181 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 O1 O 0.7715(2) 0.17756(14) 0.52735(8) 0.0815(5) Uani 1 1 d . . . N11 N 1.1665(3) 0.1133(2) 0.61754(19) 0.1244(9) Uani 1 1 d . . . N12 N 0.8073(3) 0.2783(2) 0.31909(11) 0.0978(7) Uani 1 1 d . . . C11 C 0.7362(3) 0.08565(19) 0.59403(11) 0.0613(5) Uani 1 1 d . . . C12 C 0.5738(3) 0.0501(2) 0.60943(13) 0.0796(6) Uani 1 1 d . . . H12A H 0.4839 0.0942 0.5773 0.096 Uiso 1 1 calc R . . C13 C 0.5414(3) -0.0487(3) 0.67103(16) 0.0870(7) Uani 1 1 d . . . H13A H 0.4285 -0.0729 0.6819 0.104 Uiso 1 1 calc R . . C14 C 0.6700(4) -0.1137(2) 0.71754(14) 0.0793(6) Uani 1 1 d . . . H14A H 0.6456 -0.1836 0.7596 0.095 Uiso 1 1 calc R . . C15 C 0.8334(3) -0.0783(2) 0.70361(12) 0.0705(6) Uani 1 1 d . . . H15A H 0.9224 -0.1227 0.7362 0.085 Uiso 1 1 calc R . . C16 C 0.8680(2) 0.02374(17) 0.64088(11) 0.0593(5) Uani 1 1 d . . . C17 C 1.0345(3) 0.0705(2) 0.62777(15) 0.0807(6) Uani 1 1 d . . . C21 C 0.7581(2) 0.32170(19) 0.53933(10) 0.0595(5) Uani 1 1 d . . . C22 C 0.7391(3) 0.3860(2) 0.61828(12) 0.0768(6) Uani 1 1 d . . . H22A H 0.7319 0.3302 0.6693 0.092 Uiso 1 1 calc R . . C23 C 0.7306(4) 0.5310(2) 0.62231(14) 0.1000(8) Uani 1 1 d . . . H23A H 0.7170 0.5758 0.6766 0.120 Uiso 1 1 calc R . . C24 C 0.7413(4) 0.6136(2) 0.54905(14) 0.1050(9) Uani 1 1 d . . . H24A H 0.7347 0.7144 0.5529 0.126 Uiso 1 1 calc R . . C25 C 0.7614(3) 0.5496(2) 0.47094(13) 0.0858(7) Uani 1 1 d . . . H25A H 0.7697 0.6060 0.4203 0.103 Uiso 1 1 calc R . . C26 C 0.7697(2) 0.4031(2) 0.46540(10) 0.0628(5) Uani 1 1 d . . . C27 C 0.7912(3) 0.3333(2) 0.38393(12) 0.0715(6) 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 O1 0.1398(13) 0.0591(8) 0.0472(7) 0.0062(6) 0.0229(7) 0.0163(8) N11 0.0896(16) 0.0956(16) 0.190(3) 0.0158(16) 0.0245(16) -0.0046(13) N12 0.172(2) 0.0726(12) 0.0502(10) -0.0019(9) 0.0169(11) -0.0086(12) C11 0.0896(14) 0.0516(10) 0.0435(9) -0.0024(8) 0.0112(9) 0.0048(9) C12 0.0855(16) 0.0909(16) 0.0623(12) -0.0065(11) 0.0012(11) 0.0043(12) C13 0.0890(16) 0.0944(17) 0.0790(15) -0.0163(13) 0.0192(13) -0.0182(13) C14 0.120(2) 0.0570(12) 0.0627(12) -0.0031(10) 0.0226(13) -0.0151(12) C15 0.1020(17) 0.0516(10) 0.0578(11) -0.0008(8) 0.0022(10) 0.0045(10) C16 0.0759(13) 0.0464(9) 0.0560(10) -0.0051(8) 0.0071(9) 0.0005(9) C17 0.0850(17) 0.0607(12) 0.0966(16) 0.0018(11) 0.0094(13) 0.0027(12) C21 0.0761(12) 0.0560(11) 0.0461(10) 0.0005(8) 0.0009(8) 0.0047(9) C22 0.1204(17) 0.0668(13) 0.0434(10) -0.0006(9) 0.0049(10) 0.0040(11) C23 0.174(3) 0.0711(15) 0.0558(13) -0.0163(11) 0.0119(14) -0.0002(15) C24 0.191(3) 0.0553(13) 0.0694(14) -0.0063(11) 0.0100(15) -0.0052(14) C25 0.142(2) 0.0605(13) 0.0547(11) 0.0040(9) -0.0004(12) -0.0090(12) C26 0.0818(13) 0.0613(11) 0.0448(10) -0.0006(8) -0.0016(8) -0.0051(9) C27 0.1107(16) 0.0581(11) 0.0456(10) 0.0055(9) 0.0036(10) -0.0097(11) _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 O1 C21 1.371(2) . ? O1 C11 1.382(2) . ? N11 C17 1.142(3) . ? N12 C27 1.140(2) . ? C11 C12 1.367(3) . ? C11 C16 1.381(3) . ? C12 C13 1.362(3) . ? C12 H12A 0.9500 . ? C13 C14 1.371(3) . ? C13 H13A 0.9500 . ? C14 C15 1.370(3) . ? C14 H14A 0.9500 . ? C15 C16 1.399(3) . ? C15 H15A 0.9500 . ? C16 C17 1.420(3) . ? C21 C22 1.376(2) . ? C21 C26 1.382(2) . ? C22 C23 1.365(3) . ? C22 H22A 0.9500 . ? C23 C24 1.379(3) . ? C23 H23A 0.9500 . ? C24 C25 1.364(3) . ? C24 H24A 0.9500 . ? C25 C26 1.380(3) . ? C25 H25A 0.9500 . ? C26 C27 1.437(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 C21 O1 C11 119.75(13) . . ? C12 C11 C16 120.79(18) . . ? C12 C11 O1 120.37(18) . . ? C16 C11 O1 118.72(18) . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C11 C16 C15 119.04(19) . . ? C11 C16 C17 119.39(18) . . ? C15 C16 C17 121.48(19) . . ? N11 C17 C16 177.4(2) . . ? O1 C21 C22 124.40(16) . . ? O1 C21 C26 115.25(15) . . ? C22 C21 C26 120.33(18) . . ? C23 C22 C21 119.04(18) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 121.27(19) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C25 C24 C23 119.5(2) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.10(19) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 119.70(17) . . ? C25 C26 C27 121.14(17) . . ? C21 C26 C27 119.16(17) . . ? N12 C27 C26 179.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 O1 C11 C12 81.3(2) . . . . ? C21 O1 C11 C16 -102.8(2) . . . . ? C16 C11 C12 C13 -0.8(3) . . . . ? O1 C11 C12 C13 175.06(17) . . . . ? C11 C12 C13 C14 -0.3(3) . . . . ? C12 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C12 C11 C16 C15 1.2(3) . . . . ? O1 C11 C16 C15 -174.72(15) . . . . ? C12 C11 C16 C17 -175.39(18) . . . . ? O1 C11 C16 C17 8.7(2) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C14 C15 C16 C17 176.01(18) . . . . ? C11 C16 C17 N11 49(6) . . . . ? C15 C16 C17 N11 -127(6) . . . . ? C11 O1 C21 C22 11.7(3) . . . . ? C11 O1 C21 C26 -170.09(17) . . . . ? O1 C21 C22 C23 178.6(2) . . . . ? C26 C21 C22 C23 0.5(3) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C22 C23 C24 C25 -0.3(4) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C24 C25 C26 C21 -0.2(3) . . . . ? C24 C25 C26 C27 -179.8(2) . . . . ? O1 C21 C26 C25 -178.58(19) . . . . ? C22 C21 C26 C25 -0.3(3) . . . . ? O1 C21 C26 C27 1.1(3) . . . . ? C22 C21 C26 C27 179.37(19) . . . . ? C25 C26 C27 N12 -60(30) . . . . ? C21 C26 C27 N12 121(30) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.165 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.032 _database_code_depnum_ccdc_archive 'CCDC 895074' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_w1 #TrackingRef '1-AgOTf-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H8 Ag F3 N2 O4 S' _chemical_formula_weight 477.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.1665(10) _cell_length_b 18.453(4) _cell_length_c 18.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1730.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8244 _exptl_absorpt_correction_T_max 0.9361 _exptl_absorpt_process_details 'blessing, Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4900 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1510 _reflns_number_gt 1263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+6.6176P] 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 -0.03(14) _refine_ls_number_reflns 1510 _refine_ls_number_parameters 130 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1935 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 1.00158(7) 0.7500 0.0923(5) Uani 1 2 d S . . O1 O 0.4915(15) 1.0000 1.0000 0.088(3) Uani 1 2 d S . . N1 N 0.7891(19) 1.0533(5) 0.8381(5) 0.093(3) Uani 1 1 d . . . C1 C 0.6280(19) 1.0743(5) 0.8786(5) 0.068(2) Uani 1 1 d . . . C2 C 0.4327(16) 1.1022(5) 0.9249(4) 0.062(2) Uani 1 1 d . . . C3 C 0.305(2) 1.1673(5) 0.9082(6) 0.079(3) Uani 1 1 d . . . H3A H 0.3538 1.1946 0.8674 0.095 Uiso 1 1 calc R . . C4 C 0.109(2) 1.1896(6) 0.9531(7) 0.084(3) Uani 1 1 d . . . H4A H 0.0236 1.2328 0.9425 0.101 Uiso 1 1 calc R . . C5 C 0.035(2) 1.1508(6) 1.0125(6) 0.086(3) Uani 1 1 d . . . H5A H -0.0995 1.1675 1.0420 0.103 Uiso 1 1 calc R . . C6 C 0.157(2) 1.0869(7) 1.0294(5) 0.082(3) Uani 1 1 d . . . H6A H 0.1083 1.0608 1.0710 0.098 Uiso 1 1 calc R . . C7 C 0.3533(17) 1.0613(5) 0.9837(4) 0.065(2) Uani 1 1 d . . . O2 O 0.6859(14) 0.9183(4) 0.7099(4) 0.0867(11) Uani 1 1 d . . . S1 S 0.5344(11) 0.8822(3) 0.7809(3) 0.0867(11) Uani 0.50 1 d P . . O3 O 0.696(3) 0.8502(10) 0.8363(9) 0.0867(11) Uani 0.50 1 d P . . C8 C 0.5000 0.8025(11) 0.7500 0.160(5) Uani 1 2 d SDU . . F3 F 0.329(5) 0.7693(12) 0.7943(12) 0.158(6) Uani 0.50 1 d PDU . . F1 F 0.326(4) 0.8098(11) 0.6866(10) 0.165(6) Uani 0.50 1 d PDU . . F2 F 0.648(5) 0.7511(12) 0.7254(13) 0.160(6) Uani 0.50 1 d PDU . . 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 0.0843(7) 0.1076(8) 0.0850(7) 0.000 0.0325(5) 0.000 O1 0.060(4) 0.108(7) 0.097(6) 0.035(6) 0.000 0.000 N1 0.091(6) 0.092(6) 0.095(6) -0.024(5) 0.050(5) -0.010(5) C1 0.071(5) 0.066(5) 0.066(5) -0.001(4) 0.002(4) -0.015(4) C2 0.054(5) 0.069(5) 0.062(4) -0.011(4) 0.002(4) -0.014(4) C3 0.087(6) 0.066(5) 0.085(6) -0.009(5) 0.011(5) -0.013(5) C4 0.077(6) 0.068(6) 0.109(8) -0.019(5) 0.013(6) 0.001(5) C5 0.072(6) 0.094(7) 0.091(7) -0.028(5) 0.013(6) 0.003(6) C6 0.072(6) 0.121(9) 0.052(4) -0.005(5) 0.013(4) -0.018(6) C7 0.061(5) 0.083(6) 0.050(5) -0.004(4) 0.000(3) -0.011(4) O2 0.074(2) 0.109(3) 0.0769(18) 0.0029(19) -0.018(2) -0.016(2) S1 0.074(2) 0.109(3) 0.0769(18) 0.0029(19) -0.018(2) -0.016(2) O3 0.074(2) 0.109(3) 0.0769(18) 0.0029(19) -0.018(2) -0.016(2) C8 0.204(12) 0.095(8) 0.180(13) 0.000 0.007(10) 0.000 F3 0.204(12) 0.080(10) 0.191(14) 0.001(8) 0.014(10) -0.019(8) F1 0.206(14) 0.110(9) 0.179(13) -0.007(8) -0.006(11) -0.007(8) F2 0.211(13) 0.085(9) 0.185(15) 0.000(8) 0.010(10) 0.008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.158(7) . ? Ag1 N1 2.158(8) 3_756 ? Ag1 O2 2.350(7) . ? Ag1 O2 2.350(7) 3_756 ? O1 C7 1.370(10) 4_577 ? O1 C7 1.370(10) . ? N1 C1 1.176(12) . ? C1 C2 1.411(13) . ? C2 C7 1.370(12) . ? C2 C3 1.402(14) . ? C3 C4 1.367(15) . ? C3 H3A 0.9300 . ? C4 C5 1.349(16) . ? C4 H4A 0.9300 . ? C5 C6 1.372(16) . ? C5 H5A 0.9300 . ? C6 C7 1.394(13) . ? C6 H6A 0.9300 . ? O2 S1 1.330(10) 3_656 ? O2 S1 1.647(10) . ? S1 S1 1.176(10) 3_656 ? S1 O2 1.330(10) 3_656 ? S1 O3 1.433(16) . ? S1 C8 1.583(19) . ? S1 F1 1.63(2) 3_656 ? O3 F1 0.86(2) 3_656 ? C8 F2 1.298(17) 3_656 ? C8 F2 1.298(17) . ? C8 F3 1.342(17) . ? C8 F3 1.342(17) 3_656 ? C8 F1 1.468(16) 3_656 ? C8 F1 1.468(16) . ? C8 S1 1.583(19) 3_656 ? F3 F2 0.50(4) 3_656 ? F1 O3 0.86(2) 3_656 ? F1 S1 1.63(2) 3_656 ? F2 F3 0.50(4) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 127.6(5) . 3_756 ? N1 Ag1 O2 99.8(3) . . ? N1 Ag1 O2 114.1(4) 3_756 . ? N1 Ag1 O2 114.1(3) . 3_756 ? N1 Ag1 O2 99.8(3) 3_756 3_756 ? O2 Ag1 O2 98.3(4) . 3_756 ? C7 O1 C7 117.2(9) 4_577 . ? C1 N1 Ag1 165.1(9) . . ? N1 C1 C2 177.4(11) . . ? C7 C2 C1 118.6(9) . . ? C7 C2 C3 120.0(8) . . ? C1 C2 C3 121.2(8) . . ? C4 C3 C2 118.5(10) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C5 C4 C3 121.8(11) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 120.4(9) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 119.5(9) . . ? C7 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? C2 C7 O1 117.8(7) . . ? C2 C7 C6 119.7(9) . . ? O1 C7 C6 122.1(8) . . ? S1 O2 S1 45.0(4) 3_656 . ? S1 O2 Ag1 151.6(6) 3_656 . ? S1 O2 Ag1 110.5(4) . . ? S1 S1 O2 82.0(6) 3_656 3_656 ? S1 S1 O3 147.7(9) 3_656 . ? O2 S1 O3 128.0(9) 3_656 . ? S1 S1 C8 68.2(3) 3_656 . ? O2 S1 C8 114.4(5) 3_656 . ? O3 S1 C8 86.1(8) . . ? S1 S1 F1 118.7(7) 3_656 3_656 ? O2 S1 F1 138.2(10) 3_656 3_656 ? O3 S1 F1 31.8(8) . 3_656 ? C8 S1 F1 54.3(7) . 3_656 ? S1 S1 O2 53.1(5) 3_656 . ? O2 S1 O2 107.6(7) 3_656 . ? O3 S1 O2 116.0(7) . . ? C8 S1 O2 98.8(4) . . ? F1 S1 O2 113.8(9) 3_656 . ? F1 O3 S1 86.8(18) 3_656 . ? F2 C8 F2 86(2) 3_656 . ? F2 C8 F3 22.0(17) 3_656 . ? F2 C8 F3 105.2(16) . . ? F2 C8 F3 105.2(16) 3_656 3_656 ? F2 C8 F3 22.0(17) . 3_656 ? F3 C8 F3 126(3) . 3_656 ? F2 C8 F1 99.2(14) 3_656 3_656 ? F2 C8 F1 88.6(18) . 3_656 ? F3 C8 F1 88.6(14) . 3_656 ? F3 C8 F1 96.2(14) 3_656 3_656 ? F2 C8 F1 88.6(18) 3_656 . ? F2 C8 F1 99.2(14) . . ? F3 C8 F1 96.2(14) . . ? F3 C8 F1 88.6(14) 3_656 . ? F1 C8 F1 169(2) 3_656 . ? F2 C8 S1 128.5(11) 3_656 . ? F2 C8 S1 137.2(14) . . ? F3 C8 S1 106.6(12) . . ? F3 C8 S1 124.1(15) 3_656 . ? F1 C8 S1 64.4(10) 3_656 . ? F1 C8 S1 105.1(13) . . ? F2 C8 S1 137.2(13) 3_656 3_656 ? F2 C8 S1 128.5(11) . 3_656 ? F3 C8 S1 124.1(14) . 3_656 ? F3 C8 S1 106.6(12) 3_656 3_656 ? F1 C8 S1 105.1(13) 3_656 3_656 ? F1 C8 S1 64.4(10) . 3_656 ? S1 C8 S1 43.6(6) . 3_656 ? F2 F3 C8 74(3) 3_656 . ? O3 F1 C8 122(2) 3_656 . ? O3 F1 S1 61.4(16) 3_656 3_656 ? C8 F1 S1 61.2(11) . 3_656 ? F3 F2 C8 84(3) 3_656 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.840 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 895068' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_w2 #TrackingRef '2-AgOTf-2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H8 Ag F3 N2 O4 S' _chemical_formula_weight 477.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.093(4) _cell_length_b 12.530(4) _cell_length_c 12.330(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.515(6) _cell_angle_gamma 90.00 _cell_volume 1710.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7458 _exptl_absorpt_correction_T_max 0.8994 _exptl_absorpt_process_details 'blessing, Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17879 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3023 _reflns_number_gt 2713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.7084P] 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 3023 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.113096(19) 0.870541(17) 1.121559(16) 0.05646(10) Uani 1 1 d . . . S1 S 0.18048(5) 1.11008(5) 0.99994(5) 0.04023(15) Uani 1 1 d . . . F1 F 0.41484(15) 1.10350(17) 1.01398(18) 0.0836(6) Uani 1 1 d . . . F2 F 0.32971(18) 0.97384(18) 0.9249(2) 0.1024(8) Uani 1 1 d . . . F3 F 0.3370(2) 1.1276(2) 0.85405(18) 0.1083(9) Uani 1 1 d . . . O1 O 0.18061(18) 1.04799(17) 1.09713(16) 0.0651(5) Uani 1 1 d . . . O2 O 0.1867(2) 1.22175(16) 1.01890(19) 0.0709(6) Uani 1 1 d . . . O3 O -0.09563(17) 0.9246(2) 1.08447(17) 0.0735(6) Uani 1 1 d . . . O11 O 0.25220(15) 0.98191(14) 1.54105(13) 0.0496(4) Uani 1 1 d . . . N1 N 0.1251(2) 0.86682(18) 1.3021(2) 0.0598(6) Uani 1 1 d . . . N2 N 0.1472(2) 0.7423(2) 1.00575(19) 0.0587(6) Uani 1 1 d . . . C1 C 0.3236(2) 1.0766(3) 0.9457(2) 0.0601(7) Uani 1 1 d . . . C11 C 0.1073(2) 0.87294(18) 1.3915(2) 0.0469(6) Uani 1 1 d . . . C12 C 0.0779(2) 0.87818(18) 1.5032(2) 0.0425(5) Uani 1 1 d . . . C13 C -0.0282(2) 0.8314(2) 1.5348(3) 0.0584(7) Uani 1 1 d . . . H13A H -0.0803 0.7974 1.4839 0.070 Uiso 1 1 calc R . . C14 C -0.0552(3) 0.8359(3) 1.6422(3) 0.0701(8) Uani 1 1 d . . . H14A H -0.1256 0.8043 1.6640 0.084 Uiso 1 1 calc R . . C15 C 0.0206(3) 0.8866(3) 1.7168(3) 0.0679(8) Uani 1 1 d . . . H15A H 0.0014 0.8890 1.7892 0.081 Uiso 1 1 calc R . . C16 C 0.1251(3) 0.9344(2) 1.6864(2) 0.0564(7) Uani 1 1 d . . . H16A H 0.1759 0.9694 1.7376 0.068 Uiso 1 1 calc R . . C17 C 0.1536(2) 0.92980(19) 1.5797(2) 0.0426(5) Uani 1 1 d . . . C21 C 0.3824(2) 1.1682(2) 1.5402(2) 0.0455(5) Uani 1 1 d . . . C22 C 0.4270(2) 1.07634(19) 1.60053(18) 0.0400(5) Uani 1 1 d . . . C23 C 0.5409(2) 1.0818(2) 1.6545(2) 0.0515(6) Uani 1 1 d . . . H23A H 0.5872 1.1435 1.6510 0.062 Uiso 1 1 calc R . . C24 C 0.5841(2) 0.9955(2) 1.7126(2) 0.0588(7) Uani 1 1 d . . . H24A H 0.6598 0.9984 1.7493 0.071 Uiso 1 1 calc R . . C25 C 0.5153(3) 0.9042(2) 1.7168(2) 0.0550(7) Uani 1 1 d . . . H25A H 0.5449 0.8463 1.7574 0.066 Uiso 1 1 calc R . . C26 C 0.4041(2) 0.8970(2) 1.6624(2) 0.0487(6) Uani 1 1 d . . . H26A H 0.3593 0.8345 1.6648 0.058 Uiso 1 1 calc R . . C27 C 0.3595(2) 0.98403(19) 1.60389(17) 0.0400(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 Ag1 0.06031(16) 0.05639(16) 0.05159(15) -0.00888(9) -0.00543(10) -0.00209(9) S1 0.0346(3) 0.0461(3) 0.0400(3) -0.0027(2) 0.0019(2) 0.0005(2) F1 0.0387(9) 0.1140(15) 0.0964(14) -0.0181(12) -0.0096(9) -0.0040(9) F2 0.0736(12) 0.0931(15) 0.141(2) -0.0530(14) 0.0114(13) 0.0214(11) F3 0.0901(15) 0.175(3) 0.0642(13) 0.0037(13) 0.0355(12) -0.0242(14) O1 0.0730(13) 0.0680(13) 0.0551(11) 0.0126(10) 0.0092(10) -0.0119(10) O2 0.0785(14) 0.0471(11) 0.0873(15) -0.0054(10) 0.0072(12) 0.0089(10) O3 0.0404(10) 0.1140(18) 0.0644(13) -0.0250(12) -0.0098(9) 0.0037(11) O11 0.0492(9) 0.0568(10) 0.0414(9) 0.0043(8) -0.0090(7) -0.0133(8) N1 0.0732(16) 0.0610(15) 0.0433(14) -0.0025(10) -0.0129(11) -0.0053(11) N2 0.0596(14) 0.0548(14) 0.0613(14) -0.0120(12) 0.0017(11) 0.0021(11) C1 0.0426(14) 0.077(2) 0.0612(18) -0.0148(15) 0.0052(13) -0.0028(13) C11 0.0466(14) 0.0409(13) 0.0510(16) -0.0008(11) -0.0132(11) -0.0016(10) C12 0.0402(13) 0.0387(12) 0.0477(14) -0.0017(10) -0.0043(10) 0.0056(9) C13 0.0427(14) 0.0593(17) 0.0720(19) -0.0001(14) -0.0055(13) -0.0018(12) C14 0.0454(15) 0.079(2) 0.087(2) 0.0104(18) 0.0165(16) 0.0030(15) C15 0.0643(19) 0.080(2) 0.0617(19) -0.0024(15) 0.0201(16) 0.0148(16) C16 0.0587(16) 0.0619(17) 0.0485(15) -0.0112(13) 0.0032(12) 0.0024(13) C17 0.0423(13) 0.0398(12) 0.0453(13) -0.0024(10) -0.0011(10) 0.0032(10) C21 0.0424(13) 0.0503(14) 0.0440(13) -0.0010(12) 0.0032(10) -0.0061(11) C22 0.0414(12) 0.0453(13) 0.0335(11) 0.0001(10) 0.0037(9) 0.0004(10) C23 0.0456(14) 0.0602(16) 0.0483(14) 0.0003(12) 0.0005(11) -0.0098(12) C24 0.0431(14) 0.0771(19) 0.0549(16) 0.0026(14) -0.0072(12) 0.0043(13) C25 0.0597(17) 0.0550(15) 0.0501(15) 0.0052(12) 0.0020(13) 0.0145(13) C26 0.0587(16) 0.0407(13) 0.0463(14) -0.0021(11) -0.0005(12) -0.0003(11) C27 0.0424(12) 0.0466(13) 0.0306(11) -0.0049(9) -0.0001(9) 0.0004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.198(2) . ? Ag1 N1 2.223(3) . ? Ag1 O1 2.371(2) . ? Ag1 O3 2.429(2) . ? S1 O2 1.420(2) . ? S1 O3 1.427(2) 3_577 ? S1 O1 1.429(2) . ? S1 C1 1.809(3) . ? F1 C1 1.320(3) . ? F2 C1 1.316(4) . ? F3 C1 1.314(4) . ? O3 S1 1.427(2) 3_577 ? O11 C27 1.380(3) . ? O11 C17 1.384(3) . ? N1 C11 1.134(4) . ? N2 C21 1.125(3) 2_547 ? C11 C12 1.436(4) . ? C12 C17 1.385(3) . ? C12 C13 1.392(4) . ? C13 C14 1.376(4) . ? C13 H13A 0.9300 . ? C14 C15 1.365(5) . ? C14 H14A 0.9300 . ? C15 C16 1.377(4) . ? C15 H15A 0.9300 . ? C16 C17 1.372(4) . ? C16 H16A 0.9300 . ? C21 N2 1.125(3) 2_557 ? C21 C22 1.442(4) . ? C22 C27 1.380(3) . ? C22 C23 1.393(3) . ? C23 C24 1.368(4) . ? C23 H23A 0.9300 . ? C24 C25 1.377(4) . ? C24 H24A 0.9300 . ? C25 C26 1.371(4) . ? C25 H25A 0.9300 . ? C26 C27 1.382(3) . ? C26 H26A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 129.29(9) . . ? N2 Ag1 O1 122.34(8) . . ? N1 Ag1 O1 98.45(8) . . ? N2 Ag1 O3 106.35(8) . . ? N1 Ag1 O3 101.08(9) . . ? O1 Ag1 O3 91.12(8) . . ? O2 S1 O3 116.30(15) . 3_577 ? O2 S1 O1 113.64(13) . . ? O3 S1 O1 114.37(14) 3_577 . ? O2 S1 C1 104.75(14) . . ? O3 S1 C1 102.37(13) 3_577 . ? O1 S1 C1 103.19(14) . . ? S1 O1 Ag1 129.28(13) . . ? S1 O3 Ag1 129.11(13) 3_577 . ? C27 O11 C17 119.24(18) . . ? C11 N1 Ag1 165.7(2) . . ? C21 N2 Ag1 150.9(2) 2_547 . ? F3 C1 F2 107.3(3) . . ? F3 C1 F1 107.5(3) . . ? F2 C1 F1 109.1(3) . . ? F3 C1 S1 110.7(2) . . ? F2 C1 S1 110.9(2) . . ? F1 C1 S1 111.2(2) . . ? N1 C11 C12 176.6(3) . . ? C17 C12 C13 119.6(2) . . ? C17 C12 C11 120.7(2) . . ? C13 C12 C11 119.7(2) . . ? C14 C13 C12 119.3(3) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C17 C16 C15 119.4(3) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C16 C17 O11 123.0(2) . . ? C16 C17 C12 120.5(2) . . ? O11 C17 C12 116.4(2) . . ? N2 C21 C22 176.6(3) 2_557 . ? C27 C22 C23 120.3(2) . . ? C27 C22 C21 121.0(2) . . ? C23 C22 C21 118.7(2) . . ? C24 C23 C22 119.3(3) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 121.3(3) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C27 119.1(2) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? C22 C27 O11 116.8(2) . . ? C22 C27 C26 119.9(2) . . ? O11 C27 C26 123.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Ag1 158.95(14) . . . . ? O3 S1 O1 Ag1 22.1(2) 3_577 . . . ? C1 S1 O1 Ag1 -88.21(17) . . . . ? N2 Ag1 O1 S1 40.96(19) . . . . ? N1 Ag1 O1 S1 -170.64(16) . . . . ? O3 Ag1 O1 S1 -69.26(16) . . . . ? N2 Ag1 O3 S1 -5.0(2) . . . 3_577 ? N1 Ag1 O3 S1 -141.86(19) . . . 3_577 ? O1 Ag1 O3 S1 119.3(2) . . . 3_577 ? N2 Ag1 N1 C11 -126.6(8) . . . . ? O1 Ag1 N1 C11 88.3(9) . . . . ? O3 Ag1 N1 C11 -4.5(9) . . . . ? N1 Ag1 N2 C21 79.5(5) . . . 2_547 ? O1 Ag1 N2 C21 -142.6(4) . . . 2_547 ? O3 Ag1 N2 C21 -40.4(5) . . . 2_547 ? O2 S1 C1 F3 -61.3(2) . . . . ? O3 S1 C1 F3 60.5(3) 3_577 . . . ? O1 S1 C1 F3 179.5(2) . . . . ? O2 S1 C1 F2 179.7(2) . . . . ? O3 S1 C1 F2 -58.5(3) 3_577 . . . ? O1 S1 C1 F2 60.5(2) . . . . ? O2 S1 C1 F1 58.2(3) . . . . ? O3 S1 C1 F1 179.9(2) 3_577 . . . ? O1 S1 C1 F1 -61.0(3) . . . . ? Ag1 N1 C11 C12 42(5) . . . . ? N1 C11 C12 C17 -171(4) . . . . ? N1 C11 C12 C13 9(5) . . . . ? C17 C12 C13 C14 -0.9(4) . . . . ? C11 C12 C13 C14 179.4(3) . . . . ? C12 C13 C14 C15 0.6(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 -0.7(5) . . . . ? C15 C16 C17 O11 175.3(3) . . . . ? C15 C16 C17 C12 0.3(4) . . . . ? C27 O11 C17 C16 39.7(3) . . . . ? C27 O11 C17 C12 -145.1(2) . . . . ? C13 C12 C17 C16 0.5(4) . . . . ? C11 C12 C17 C16 -179.9(2) . . . . ? C13 C12 C17 O11 -174.9(2) . . . . ? C11 C12 C17 O11 4.8(3) . . . . ? N2 C21 C22 C27 -175(5) 2_557 . . . ? N2 C21 C22 C23 4(5) 2_557 . . . ? C27 C22 C23 C24 -1.3(4) . . . . ? C21 C22 C23 C24 179.6(2) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C23 C24 C25 C26 0.9(4) . . . . ? C24 C25 C26 C27 -1.2(4) . . . . ? C23 C22 C27 O11 -174.7(2) . . . . ? C21 C22 C27 O11 4.3(3) . . . . ? C23 C22 C27 C26 1.0(3) . . . . ? C21 C22 C27 C26 -179.9(2) . . . . ? C17 O11 C27 C22 -143.7(2) . . . . ? C17 O11 C27 C26 40.7(3) . . . . ? C25 C26 C27 C22 0.3(4) . . . . ? C25 C26 C27 O11 175.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.292 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 895069' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef '4-AgOTf-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H34 Ag3 F9 N8 O14 S3' _chemical_formula_weight 1669.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.141(3) _cell_length_b 15.663(3) _cell_length_c 16.402(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.459(6) _cell_angle_gamma 90.00 _cell_volume 3446.0(12) _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 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.8532 _exptl_absorpt_process_details 'blessing, Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48860 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 24.50 _reflns_number_total 11291 _reflns_number_gt 8017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1620P)^2^+1.6772P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11291 _refine_ls_number_parameters 881 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2550 _refine_ls_wR_factor_gt 0.2318 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.139 _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 0.77344(5) 0.74326(4) 1.18993(4) 0.0490(3) Uani 1 1 d D A . Ag2 Ag 0.55116(5) 0.92599(4) 1.09090(5) 0.0571(3) Uani 1 1 d D . . Ag3 Ag 0.38048(4) 0.47658(4) 0.94599(4) 0.0437(2) Uani 1 1 d . . . S2 S 0.10552(14) 0.41227(13) 0.85856(13) 0.0435(5) Uani 1 1 d DU . . S3 S 0.6158(2) 0.7887(2) 0.45361(16) 0.0765(9) Uani 1 1 d . . . O1 O 0.7708(4) 0.9583(3) 0.8638(4) 0.0460(14) Uani 1 1 d . . . O2 O 0.4415(4) 0.8451(4) 0.7848(4) 0.0596(17) Uani 1 1 d . . . O3 O 0.6737(4) 0.2838(3) 1.0166(4) 0.0489(15) Uani 1 1 d . . . O4 O 0.5051(4) 0.4878(4) 1.2908(3) 0.0502(15) Uani 1 1 d . . . O5 O 0.6670(5) 0.8532(4) 1.2287(4) 0.0651(18) Uani 1 1 d D . . H5D H 0.7163(13) 0.8798(13) 1.2604(15) 0.098 Uiso 1 1 d D . . H5E H 0.6456(17) 0.8200(14) 1.2582(16) 0.098 Uiso 1 1 d D . . O13 O 0.5781(4) 0.8047(4) 0.5175(4) 0.0548(15) Uani 1 1 d . . . O14 O 0.5814(7) 0.6910(6) 0.4408(6) 0.097(3) Uani 1 1 d . . . N1 N 0.7949(5) 0.8569(5) 1.0825(4) 0.056(2) Uani 1 1 d . . . N2 N 0.5563(6) 1.0538(5) 0.8457(6) 0.068(2) Uani 1 1 d . . . N3 N 0.5558(5) 0.8533(4) 0.9949(5) 0.0488(18) Uani 1 1 d . . . N4 N 0.3838(5) 0.6060(4) 0.8453(5) 0.0448(16) Uani 1 1 d . . . N5 N 0.4420(5) 0.3634(4) 0.9261(4) 0.0427(16) Uani 1 1 d . . . N6 N 0.6607(5) 0.0513(4) 1.0841(5) 0.056(2) Uani 1 1 d . . . N7 N 0.3662(5) 0.4828(4) 1.0750(4) 0.0452(16) Uani 1 1 d . . . N8 N 0.7193(5) 0.6229(5) 1.2706(4) 0.0521(19) Uani 1 1 d . . . F4 F 0.0903(7) 0.4572(5) 0.9968(6) 0.133(3) Uani 1 1 d U . . F5 F -0.0355(4) 0.3727(5) 0.9383(5) 0.104(2) Uani 1 1 d U . . F6 F 0.0949(6) 0.3237(5) 1.0116(5) 0.106(2) Uani 1 1 d U . . F7 F 0.7849(8) 0.8551(9) 0.5151(14) 0.314(13) Uani 1 1 d . . . F8 F 0.7682(7) 0.7247(9) 0.5773(7) 0.174(6) Uani 1 1 d . . . F9 F 0.7859(5) 0.7496(4) 0.4514(6) 0.114(3) Uani 1 1 d . . . C2 C 0.0588(6) 0.3989(6) 0.9504(6) 0.057(2) Uani 1 1 d U . . C3 C 0.7424(9) 0.7710(11) 0.5041(14) 0.117(6) Uani 1 1 d . . . C11 C 0.8236(5) 0.9245(5) 1.0411(5) 0.044(2) Uani 1 1 d D . . C12 C 0.8606(5) 0.9983(5) 0.9983(5) 0.045(2) Uani 1 1 d D . . C13 C 0.9291(6) 1.0598(5) 1.0418(6) 0.051(2) Uani 1 1 d . . . H13A H 0.9533 1.0561 1.1028 0.061 Uiso 1 1 calc R . . C14 C 0.9693(6) 1.1342(5) 0.9992(7) 0.060(3) Uani 1 1 d . . . H14A H 1.0154 1.1719 1.0370 0.072 Uiso 1 1 calc R . . C15 C 0.9436(6) 1.1525(5) 0.9068(8) 0.060(3) Uani 1 1 d . . . H15A H 0.9708 1.1987 0.8839 0.072 Uiso 1 1 calc R . . C16 C 0.8769(6) 1.0961(5) 0.8580(6) 0.044(2) Uani 1 1 d . . . H16A H 0.8546 1.1008 0.7971 0.053 Uiso 1 1 calc R . . C17 C 0.8365(5) 1.0214(4) 0.9045(5) 0.0394(19) Uani 1 1 d . . . C21 C 0.5924(7) 1.0393(5) 0.7967(7) 0.056(2) Uani 1 1 d . . . C22 C 0.6382(6) 1.0189(4) 0.7375(6) 0.0419(19) Uani 1 1 d . . . C23 C 0.5934(7) 1.0351(6) 0.6473(6) 0.054(2) Uani 1 1 d . . . H23A H 0.5294 1.0610 0.6275 0.064 Uiso 1 1 calc R . . C24 C 0.6380(7) 1.0151(6) 0.5929(6) 0.062(3) Uani 1 1 d . . . H24A H 0.6108 1.0268 0.5331 0.075 Uiso 1 1 calc R . . C25 C 0.7281(7) 0.9756(6) 0.6284(6) 0.055(2) Uani 1 1 d . . . H25A H 0.7625 0.9579 0.5901 0.066 Uiso 1 1 calc R . . C26 C 0.7761(6) 0.9583(5) 0.7191(6) 0.045(2) Uani 1 1 d . . . H26A H 0.8395 0.9313 0.7384 0.054 Uiso 1 1 calc R . . C27 C 0.7302(6) 0.9804(5) 0.7735(5) 0.0392(18) Uani 1 1 d . . . C31 C 0.5737(5) 0.8267(5) 0.9435(5) 0.0388(18) Uani 1 1 d . . . C32 C 0.5960(5) 0.7953(4) 0.8768(5) 0.0317(15) Uani 1 1 d . . . C33 C 0.6861(5) 0.7591(4) 0.8923(5) 0.0356(17) Uani 1 1 d . . . H33A H 0.7309 0.7514 0.9488 0.043 Uiso 1 1 calc R . . C34 C 0.7073(6) 0.7355(5) 0.8249(5) 0.0405(18) Uani 1 1 d . . . H34A H 0.7688 0.7076 0.8306 0.049 Uiso 1 1 calc R . . C35 C 0.6378(6) 0.7516(5) 0.7409(5) 0.0424(19) Uani 1 1 d . . . H35A H 0.6584 0.7365 0.6930 0.051 Uiso 1 1 calc R . . C36 C 0.5485(6) 0.7851(5) 0.7243(5) 0.045(2) Uani 1 1 d . . . H36A H 0.5040 0.7927 0.6677 0.054 Uiso 1 1 calc R . . C37 C 0.5272(6) 0.8065(5) 0.7923(5) 0.0405(18) Uani 1 1 d . . . C41 C 0.3522(6) 0.6683(5) 0.7912(6) 0.054(2) Uani 1 1 d DU . . C42 C 0.3115(7) 0.7384(6) 0.7270(7) 0.072(2) Uani 1 1 d DU . . C43 C 0.2171(10) 0.7281(8) 0.6699(9) 0.102(3) Uani 1 1 d U . . H43A H 0.1824 0.6759 0.6687 0.123 Uiso 1 1 calc R . . C44 C 0.1687(11) 0.7987(9) 0.6096(11) 0.121(4) Uani 1 1 d U . . H44A H 0.1032 0.7893 0.5716 0.145 Uiso 1 1 calc R . . C45 C 0.2171(11) 0.8849(9) 0.6050(10) 0.117(4) Uani 1 1 d U . . H45A H 0.1843 0.9276 0.5649 0.140 Uiso 1 1 calc R . . C46 C 0.3073(9) 0.8966(8) 0.6600(8) 0.089(3) Uani 1 1 d U . . H46A H 0.3421 0.9486 0.6604 0.107 Uiso 1 1 calc R . . C47 C 0.3535(7) 0.8264(6) 0.7217(7) 0.069(2) Uani 1 1 d U . . C51 C 0.4969(5) 0.3342(5) 0.9038(5) 0.0389(18) Uani 1 1 d . . . C52 C 0.5664(5) 0.3030(5) 0.8724(5) 0.0396(18) Uani 1 1 d . . . C53 C 0.5426(6) 0.3004(5) 0.7841(6) 0.047(2) Uani 1 1 d . . . H53A H 0.4776 0.3136 0.7471 0.056 Uiso 1 1 calc R . . C54 C 0.6160(7) 0.2782(6) 0.7536(7) 0.058(2) Uani 1 1 d . . . H54A H 0.6047 0.2746 0.6935 0.070 Uiso 1 1 calc R . . C55 C 0.7121(7) 0.2597(6) 0.8135(7) 0.063(3) Uani 1 1 d . . . H55A H 0.7648 0.2466 0.7912 0.076 Uiso 1 1 calc R . . C56 C 0.7327(6) 0.2599(5) 0.9002(6) 0.049(2) Uani 1 1 d . . . H56A H 0.7972 0.2450 0.9370 0.059 Uiso 1 1 calc R . . C57 C 0.6612(5) 0.2812(4) 0.9323(6) 0.0412(19) Uani 1 1 d . . . C61 C 0.7179(6) 0.1074(5) 1.1029(6) 0.047(2) Uani 1 1 d . . . C62 C 0.7886(6) 0.1799(5) 1.1240(6) 0.047(2) Uani 1 1 d . . . C63 C 0.8780(7) 0.1646(6) 1.1915(7) 0.064(3) Uani 1 1 d . . . H63A H 0.8923 0.1117 1.2214 0.077 Uiso 1 1 calc R . . C64 C 0.9444(8) 0.2348(6) 1.2108(10) 0.100(5) Uani 1 1 d . . . H64A H 1.0061 0.2281 1.2554 0.121 Uiso 1 1 calc R . . C65 C 0.9236(8) 0.3187(6) 1.1656(11) 0.113(6) Uani 1 1 d . . . H65A H 0.9730 0.3620 1.1819 0.136 Uiso 1 1 calc R . . C66 C 0.8338(7) 0.3364(5) 1.0997(9) 0.078(4) Uani 1 1 d . . . H66A H 0.8199 0.3906 1.0725 0.094 Uiso 1 1 calc R . . C67 C 0.7662(6) 0.2673(5) 1.0772(6) 0.049(2) Uani 1 1 d . . . C71 C 0.3531(5) 0.4855(5) 1.1401(5) 0.0386(18) Uani 1 1 d . . . C72 C 0.3324(5) 0.4899(5) 1.2170(5) 0.0414(18) Uani 1 1 d . . . C73 C 0.2346(6) 0.4977(7) 1.2171(7) 0.066(3) Uani 1 1 d . . . H73A H 0.1805 0.4992 1.1650 0.079 Uiso 1 1 calc R . . C74 C 0.2187(10) 0.5032(9) 1.2962(11) 0.104(5) Uani 1 1 d . . . H74A H 0.1525 0.5109 1.2972 0.124 Uiso 1 1 calc R . . C75 C 0.2942(11) 0.4981(12) 1.3730(9) 0.115(5) Uani 1 1 d . . . H75A H 0.2803 0.5000 1.4260 0.138 Uiso 1 1 calc R . . C76 C 0.3886(9) 0.4902(9) 1.3714(7) 0.083(4) Uani 1 1 d . . . H76A H 0.4413 0.4858 1.4242 0.099 Uiso 1 1 calc R . . C77 C 0.4103(6) 0.4884(6) 1.2977(6) 0.050(2) Uani 1 1 d . . . C81 C 0.6979(5) 0.5556(5) 1.3165(5) 0.046(2) Uani 1 1 d D . . C82 C 0.6750(6) 0.4825(6) 1.3681(5) 0.058(3) Uani 1 1 d D . . C83 C 0.7532(7) 0.4325(9) 1.4397(6) 0.086(4) Uani 1 1 d . . . H83A H 0.8207 0.4499 1.4523 0.104 Uiso 1 1 calc R . . C84 C 0.7328(8) 0.3561(10) 1.4938(7) 0.100(5) Uani 1 1 d . . . H84A H 0.7880 0.3300 1.5353 0.120 Uiso 1 1 calc R . . C85 C 0.6340(8) 0.3235(8) 1.4834(6) 0.078(3) Uani 1 1 d . . . H85A H 0.6213 0.2782 1.5171 0.093 Uiso 1 1 calc R . . C86 C 0.5563(7) 0.3663(7) 1.4167(5) 0.062(3) Uani 1 1 d . . . H86A H 0.4895 0.3480 1.4062 0.074 Uiso 1 1 calc R . . C87 C 0.5763(6) 0.4411(6) 1.3609(5) 0.051(2) Uani 1 1 d . . . S1 S 0.9422(3) 0.9023(2) 1.2998(2) 0.1125(16) Uani 1 1 d D A . C1 C 0.9960(8) 0.9166(5) 1.4082(5) 0.108(4) Uani 1 1 d DU . . F1 F 1.0930(6) 0.8832(7) 1.4206(6) 0.045(4) Uani 0.426(15) 1 d PDU A 1 F10 F 0.8663(9) 0.9563(10) 1.3905(9) 0.119(6) Uani 0.574(15) 1 d P A 3 F2 F 1.0264(5) 1.0006(4) 1.4125(4) 0.0784(18) Uani 1 1 d DU A . F3 F 0.9693(5) 0.8738(4) 1.4719(4) 0.0748(16) Uani 1 1 d DU A . O6 O 0.9069(6) 0.8155(4) 1.3023(5) 0.109(4) Uani 1 1 d D . . O7 O 0.9798(6) 0.9637(5) 1.2421(4) 0.091(3) Uani 1 1 d D . . O8 O 0.8407(6) 0.9495(6) 1.2816(7) 0.115(3) Uani 1 1 d D . . O9 O 0.1996(5) 0.4542(6) 0.8792(6) 0.106(2) Uani 1 1 d DU . . O10 O 0.0600(10) 0.4896(6) 0.8040(7) 0.131(3) Uani 1 1 d DU . . O11 O 0.0671(7) 0.3362(5) 0.8206(6) 0.106(3) Uani 1 1 d DU . . O12 O 0.5951(11) 0.8380(9) 0.3711(7) 0.170(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0442(4) 0.0607(5) 0.0444(4) -0.0197(3) 0.0175(3) -0.0169(3) Ag2 0.0525(4) 0.0492(5) 0.0840(5) -0.0455(4) 0.0420(4) -0.0137(3) Ag3 0.0349(4) 0.0382(4) 0.0549(4) -0.0185(3) 0.0096(3) 0.0076(3) S2 0.0355(10) 0.0442(11) 0.0518(11) -0.0295(9) 0.0153(9) -0.0106(8) S3 0.0546(15) 0.132(3) 0.0526(14) 0.0122(15) 0.0310(12) 0.0394(16) O1 0.052(3) 0.040(3) 0.052(3) -0.024(3) 0.025(3) -0.013(2) O2 0.037(3) 0.059(4) 0.072(4) -0.025(3) 0.001(3) 0.014(3) O3 0.034(3) 0.044(3) 0.066(4) -0.025(3) 0.012(3) 0.007(2) O4 0.025(3) 0.091(4) 0.032(3) -0.019(3) 0.006(2) -0.008(3) O5 0.066(4) 0.065(4) 0.076(4) -0.044(3) 0.039(4) -0.005(3) O13 0.050(3) 0.071(4) 0.051(3) -0.014(3) 0.026(3) 0.009(3) O14 0.101(6) 0.095(6) 0.095(6) -0.048(5) 0.030(5) -0.039(5) N1 0.036(4) 0.093(6) 0.040(4) -0.034(4) 0.015(3) -0.016(4) N2 0.072(5) 0.053(5) 0.104(7) -0.040(4) 0.065(5) -0.006(4) N3 0.041(4) 0.042(4) 0.070(5) -0.036(4) 0.027(4) -0.013(3) N4 0.042(4) 0.028(3) 0.063(4) -0.010(3) 0.015(3) 0.005(3) N5 0.034(3) 0.042(4) 0.052(4) -0.021(3) 0.014(3) 0.008(3) N6 0.048(4) 0.039(4) 0.084(5) -0.037(4) 0.026(4) -0.007(3) N7 0.047(4) 0.042(4) 0.038(4) -0.017(3) 0.000(3) -0.003(3) N8 0.035(4) 0.079(5) 0.046(4) -0.028(4) 0.018(3) -0.014(3) F4 0.171(7) 0.119(6) 0.155(7) -0.109(5) 0.118(6) -0.077(5) F5 0.046(3) 0.150(6) 0.133(6) -0.066(5) 0.051(4) -0.019(4) F6 0.122(6) 0.108(6) 0.090(5) 0.005(4) 0.034(4) 0.029(5) F7 0.124(8) 0.246(14) 0.63(3) -0.34(2) 0.210(14) -0.115(9) F8 0.099(7) 0.247(13) 0.127(7) -0.094(8) -0.034(6) 0.097(8) F9 0.069(4) 0.088(5) 0.204(9) -0.073(5) 0.072(5) -0.002(3) C2 0.038(4) 0.062(5) 0.074(5) -0.044(4) 0.020(4) -0.003(4) C3 0.036(6) 0.128(12) 0.191(17) -0.071(12) 0.042(9) 0.005(7) C11 0.026(4) 0.064(6) 0.047(4) -0.033(4) 0.017(3) -0.011(4) C12 0.027(4) 0.053(5) 0.058(5) -0.035(4) 0.020(4) 0.005(3) C13 0.030(4) 0.045(5) 0.076(6) -0.041(4) 0.012(4) 0.005(3) C14 0.033(4) 0.042(5) 0.097(8) -0.034(5) 0.009(5) 0.004(4) C15 0.029(4) 0.025(4) 0.124(9) -0.023(5) 0.023(5) -0.003(3) C16 0.033(4) 0.033(4) 0.069(5) -0.017(4) 0.021(4) 0.006(3) C17 0.028(4) 0.026(4) 0.071(5) -0.025(4) 0.024(4) -0.001(3) C21 0.062(5) 0.030(4) 0.095(7) -0.012(4) 0.053(6) -0.005(4) C22 0.049(5) 0.022(4) 0.069(5) -0.011(4) 0.039(4) 0.002(3) C23 0.048(5) 0.049(5) 0.073(6) 0.007(4) 0.032(5) 0.012(4) C24 0.061(6) 0.072(7) 0.057(6) -0.007(5) 0.022(5) 0.005(5) C25 0.052(5) 0.065(6) 0.057(5) -0.020(4) 0.032(4) -0.006(4) C26 0.040(4) 0.044(5) 0.058(5) -0.026(4) 0.024(4) -0.002(3) C27 0.038(4) 0.032(4) 0.054(5) -0.021(3) 0.024(4) -0.004(3) C31 0.032(4) 0.034(4) 0.050(5) -0.020(4) 0.013(3) -0.005(3) C32 0.035(4) 0.025(4) 0.040(4) -0.015(3) 0.019(3) -0.005(3) C33 0.036(4) 0.033(4) 0.037(4) -0.020(3) 0.010(3) -0.003(3) C34 0.041(4) 0.036(4) 0.046(4) -0.027(3) 0.017(4) -0.010(3) C35 0.053(5) 0.041(4) 0.040(4) -0.021(3) 0.023(4) -0.016(4) C36 0.055(5) 0.042(5) 0.033(4) -0.014(3) 0.004(4) -0.009(4) C37 0.037(4) 0.028(4) 0.053(5) -0.013(3) 0.008(4) -0.004(3) C41 0.036(4) 0.051(4) 0.072(5) -0.014(4) 0.011(3) 0.000(3) C42 0.048(4) 0.056(4) 0.095(5) -0.001(4) -0.001(4) 0.007(3) C43 0.072(5) 0.077(5) 0.124(6) 0.012(5) -0.018(5) -0.001(4) C44 0.087(5) 0.093(5) 0.140(6) 0.025(5) -0.023(5) -0.001(5) C45 0.087(5) 0.086(5) 0.136(6) 0.031(5) -0.024(5) 0.008(5) C46 0.065(5) 0.067(5) 0.113(6) 0.018(4) -0.003(4) 0.011(4) C47 0.047(4) 0.055(4) 0.090(5) 0.004(4) 0.002(4) 0.011(3) C51 0.030(4) 0.035(4) 0.045(4) -0.019(3) 0.002(3) 0.000(3) C52 0.031(4) 0.030(4) 0.063(5) -0.014(4) 0.023(4) 0.000(3) C53 0.043(4) 0.041(5) 0.063(5) -0.023(4) 0.026(4) 0.000(4) C54 0.061(6) 0.053(5) 0.075(6) -0.022(5) 0.040(5) -0.004(4) C55 0.056(6) 0.049(5) 0.102(8) -0.017(5) 0.050(6) 0.011(4) C56 0.035(4) 0.038(5) 0.080(6) -0.012(4) 0.026(4) 0.007(3) C57 0.033(4) 0.022(4) 0.073(6) -0.016(4) 0.023(4) -0.002(3) C61 0.037(4) 0.034(4) 0.072(6) -0.020(4) 0.020(4) 0.007(4) C62 0.032(4) 0.031(4) 0.074(6) -0.030(4) 0.010(4) 0.008(3) C63 0.042(5) 0.035(5) 0.105(8) -0.020(5) 0.008(5) 0.009(4) C64 0.050(6) 0.042(6) 0.163(13) -0.022(7) -0.032(7) 0.004(5) C65 0.042(6) 0.037(6) 0.214(16) -0.036(7) -0.026(7) 0.001(4) C66 0.047(5) 0.016(4) 0.153(11) -0.016(5) 0.004(6) 0.002(4) C67 0.031(4) 0.031(4) 0.077(6) -0.024(4) 0.004(4) 0.011(3) C71 0.028(4) 0.033(4) 0.046(5) -0.016(3) -0.001(3) -0.003(3) C72 0.030(4) 0.044(5) 0.052(5) -0.015(4) 0.015(3) -0.005(3) C73 0.024(4) 0.082(7) 0.091(7) -0.001(6) 0.018(5) 0.000(4) C74 0.074(8) 0.120(11) 0.155(14) -0.015(10) 0.091(10) 0.002(7) C75 0.079(9) 0.201(17) 0.083(9) -0.027(10) 0.052(8) 0.019(10) C76 0.065(7) 0.136(11) 0.057(6) -0.041(6) 0.033(5) -0.009(7) C77 0.035(4) 0.069(6) 0.051(5) -0.021(4) 0.023(4) -0.018(4) C81 0.026(4) 0.078(6) 0.034(4) -0.023(4) 0.010(3) -0.019(4) C82 0.030(4) 0.104(8) 0.037(4) -0.015(5) 0.004(3) -0.021(4) C83 0.036(5) 0.161(12) 0.047(5) 0.024(7) -0.009(4) -0.031(6) C84 0.050(6) 0.174(14) 0.062(7) 0.041(8) -0.001(5) -0.026(7) C85 0.055(6) 0.118(10) 0.048(5) 0.009(6) -0.002(5) -0.031(6) C86 0.050(5) 0.098(8) 0.037(4) -0.019(5) 0.014(4) -0.037(5) C87 0.032(4) 0.090(7) 0.027(4) -0.021(4) 0.004(3) -0.027(4) S1 0.120(3) 0.140(3) 0.118(3) -0.114(3) 0.096(2) -0.093(2) C1 0.147(9) 0.090(7) 0.067(6) -0.022(6) 0.006(6) -0.023(7) F1 0.017(5) 0.061(7) 0.047(6) -0.014(4) -0.002(4) 0.008(4) F10 0.064(7) 0.156(13) 0.118(11) -0.076(9) 0.002(7) 0.046(8) F2 0.093(4) 0.066(4) 0.074(4) -0.056(3) 0.024(3) -0.019(3) F3 0.082(4) 0.086(4) 0.064(3) -0.026(3) 0.033(3) 0.001(3) O6 0.092(6) 0.069(5) 0.114(6) -0.065(5) -0.041(5) 0.013(4) O7 0.101(6) 0.090(6) 0.062(4) -0.028(4) -0.001(4) 0.033(5) O8 0.059(5) 0.119(7) 0.152(9) -0.031(6) 0.011(5) 0.019(5) O9 0.061(4) 0.145(6) 0.119(5) -0.064(4) 0.040(4) -0.039(4) O10 0.168(7) 0.118(6) 0.117(6) 0.017(5) 0.056(5) 0.049(6) O11 0.128(7) 0.093(5) 0.117(6) -0.070(5) 0.067(6) -0.043(5) O12 0.205(13) 0.236(13) 0.118(8) 0.058(9) 0.121(9) 0.155(11) _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 O6 2.456(6) . ? Ag1 O5 2.498(6) . ? Ag1 N8 2.555(8) . ? Ag1 N1 2.589(9) . ? Ag2 N3 1.961(7) . ? Ag2 N2 2.119(7) 2_677 ? Ag2 N6 2.524(8) 1_565 ? Ag2 O5 2.598(7) . ? Ag3 N5 2.046(6) . ? Ag3 N7 2.191(7) . ? Ag3 O9 2.468(7) . ? Ag3 N4 2.625(7) . ? Ag3 Ag3 3.3632(13) 2_667 ? S2 O11 1.374(6) . ? S2 O9 1.424(6) . ? S2 O10 1.522(7) . ? S2 C2 1.838(10) . ? S3 O13 1.343(6) . ? S3 O12 1.504(10) . ? S3 O14 1.599(9) . ? S3 C3 1.740(14) . ? O1 C17 1.375(9) . ? O1 C27 1.451(10) . ? O2 C37 1.324(9) . ? O2 C47 1.375(11) . ? O3 C57 1.339(10) . ? O3 C67 1.394(9) . ? O4 C77 1.380(9) . ? O4 C87 1.462(10) . ? O5 H5D 0.837(10) . ? O5 H5E 0.829(10) . ? N1 C11 1.387(11) . ? N2 C21 1.103(11) . ? N2 Ag2 2.119(7) 2_677 ? N3 C31 1.042(9) . ? N4 C41 1.298(10) . ? N5 C51 1.061(9) . ? N6 C61 1.167(11) . ? N6 Ag2 2.524(7) 1_545 ? N7 C71 1.140(10) . ? N8 C81 1.384(11) . ? F4 C2 1.182(10) . ? F5 C2 1.349(10) . ? F6 C2 1.526(13) . ? F7 C3 1.435(19) . ? F8 C3 1.35(2) . ? F9 C3 1.256(17) . ? C11 C12 1.528(8) . ? C12 C13 1.392(10) . ? C12 C17 1.510(12) . ? C13 C14 1.556(14) . ? C13 H13A 0.9500 . ? C14 C15 1.471(15) . ? C14 H14A 0.9500 . ? C15 C16 1.354(11) . ? C15 H15A 0.9500 . ? C16 C17 1.599(12) . ? C16 H16A 0.9500 . ? C21 C22 1.365(12) . ? C22 C27 1.385(11) . ? C22 C23 1.436(13) . ? C23 C24 1.284(12) . ? C23 H23A 0.9500 . ? C24 C25 1.371(13) . ? C24 H24A 0.9500 . ? C25 C26 1.452(13) . ? C25 H25A 0.9500 . ? C26 C27 1.306(10) . ? C26 H26A 0.9500 . ? C31 C32 1.324(10) . ? C32 C33 1.345(10) . ? C32 C37 1.429(11) . ? C33 C34 1.287(10) . ? C33 H33A 0.9500 . ? C34 C35 1.439(11) . ? C34 H34A 0.9500 . ? C35 C36 1.313(12) . ? C35 H35A 0.9500 . ? C36 C37 1.289(11) . ? C36 H36A 0.9500 . ? C41 C42 1.504(9) . ? C42 C43 1.376(15) . ? C42 C47 1.514(14) . ? C43 C44 1.498(17) . ? C43 H43A 0.9500 . ? C44 C45 1.53(2) . ? C44 H44A 0.9500 . ? C45 C46 1.321(17) . ? C45 H45A 0.9500 . ? C46 C47 1.497(14) . ? C46 H46A 0.9500 . ? C51 C52 1.337(11) . ? C52 C53 1.381(12) . ? C52 C57 1.430(11) . ? C53 C54 1.332(12) . ? C53 H53A 0.9500 . ? C54 C55 1.432(14) . ? C54 H54A 0.9500 . ? C55 C56 1.358(14) . ? C55 H55A 0.9500 . ? C56 C57 1.321(11) . ? C56 H56A 0.9500 . ? C61 C62 1.480(11) . ? C62 C63 1.412(12) . ? C62 C67 1.553(12) . ? C63 C64 1.416(14) . ? C63 H63A 0.9500 . ? C64 C65 1.491(17) . ? C64 H64A 0.9500 . ? C65 C66 1.410(15) . ? C65 H65A 0.9500 . ? C66 C67 1.414(12) . ? C66 H66A 0.9500 . ? C71 C72 1.384(12) . ? C72 C73 1.389(11) . ? C72 C77 1.430(11) . ? C73 C74 1.387(17) . ? C73 H73A 0.9500 . ? C74 C75 1.37(2) . ? C74 H74A 0.9500 . ? C75 C76 1.349(17) . ? C75 H75A 0.9500 . ? C76 C77 1.338(13) . ? C76 H76A 0.9500 . ? C81 C82 1.519(9) . ? C82 C87 1.509(10) . ? C82 C83 1.547(13) . ? C83 C84 1.571(16) . ? C83 H83A 0.9500 . ? C84 C85 1.446(14) . ? C84 H84A 0.9500 . ? C85 C86 1.446(15) . ? C85 H85A 0.9500 . ? C86 C87 1.567(13) . ? C86 H86A 0.9500 . ? S1 O6 1.453(7) . ? S1 O8 1.557(7) . ? S1 O7 1.557(8) . ? S1 C1 1.713(8) . ? C1 F2 1.380(7) . ? C1 F3 1.390(7) . ? C1 F1 1.422(9) . ? C1 F10 1.871(15) . ? F10 O8 1.709(17) . ? 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 O6 Ag1 O5 82.7(2) . . ? O6 Ag1 N8 103.7(3) . . ? O5 Ag1 N8 94.2(2) . . ? O6 Ag1 N1 88.1(3) . . ? O5 Ag1 N1 84.8(2) . . ? N8 Ag1 N1 168.0(2) . . ? N3 Ag2 N2 133.8(3) . 2_677 ? N3 Ag2 N6 103.9(3) . 1_565 ? N2 Ag2 N6 116.8(3) 2_677 1_565 ? N3 Ag2 O5 105.8(3) . . ? N2 Ag2 O5 89.5(3) 2_677 . ? N6 Ag2 O5 98.8(2) 1_565 . ? N5 Ag3 N7 111.5(3) . . ? N5 Ag3 O9 103.8(3) . . ? N7 Ag3 O9 92.0(3) . . ? N5 Ag3 N4 118.4(2) . . ? N7 Ag3 N4 126.8(2) . . ? O9 Ag3 N4 93.0(3) . . ? N5 Ag3 Ag3 82.29(18) . 2_667 ? N7 Ag3 Ag3 82.31(18) . 2_667 ? O9 Ag3 Ag3 172.9(2) . 2_667 ? N4 Ag3 Ag3 87.02(15) . 2_667 ? O11 S2 O9 135.4(6) . . ? O11 S2 O10 113.0(7) . . ? O9 S2 O10 87.9(7) . . ? O11 S2 C2 94.5(5) . . ? O9 S2 C2 114.1(5) . . ? O10 S2 C2 112.2(5) . . ? O13 S3 O12 126.4(4) . . ? O13 S3 O14 95.9(5) . . ? O12 S3 O14 114.1(8) . . ? O13 S3 C3 105.2(7) . . ? O12 S3 C3 112.8(9) . . ? O14 S3 C3 97.8(7) . . ? C17 O1 C27 108.2(6) . . ? C37 O2 C47 123.8(7) . . ? C57 O3 C67 121.2(6) . . ? C77 O4 C87 112.6(6) . . ? Ag1 O5 Ag2 110.2(2) . . ? Ag1 O5 H5D 93.0(16) . . ? Ag2 O5 H5D 119.6(18) . . ? Ag1 O5 H5E 94.4(17) . . ? Ag2 O5 H5E 122.4(18) . . ? H5D O5 H5E 109.7(16) . . ? C11 N1 Ag1 166.9(5) . . ? C21 N2 Ag2 163.2(9) . 2_677 ? C31 N3 Ag2 163.9(7) . . ? C41 N4 Ag3 159.9(6) . . ? C51 N5 Ag3 145.3(7) . . ? C61 N6 Ag2 163.1(8) . 1_545 ? C71 N7 Ag3 176.1(6) . . ? C81 N8 Ag1 175.4(5) . . ? F4 C2 F5 118.9(8) . . ? F4 C2 F6 101.1(9) . . ? F5 C2 F6 88.4(8) . . ? F4 C2 S2 106.2(8) . . ? F5 C2 S2 120.7(7) . . ? F6 C2 S2 119.7(5) . . ? F9 C3 F8 114.5(12) . . ? F9 C3 F7 93.1(13) . . ? F8 C3 F7 113.4(17) . . ? F9 C3 S3 111.7(14) . . ? F8 C3 S3 117.1(11) . . ? F7 C3 S3 104.0(12) . . ? N1 C11 C12 177.2(7) . . ? C13 C12 C17 104.7(7) . . ? C13 C12 C11 124.9(8) . . ? C17 C12 C11 130.5(6) . . ? C12 C13 C14 125.6(8) . . ? C12 C13 H13A 117.2 . . ? C14 C13 H13A 117.2 . . ? C15 C14 C13 127.1(7) . . ? C15 C14 H14A 116.5 . . ? C13 C14 H14A 116.5 . . ? C16 C15 C14 112.4(9) . . ? C16 C15 H15A 123.8 . . ? C14 C15 H15A 123.8 . . ? C15 C16 C17 118.9(9) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? O1 C17 C12 102.9(6) . . ? O1 C17 C16 125.6(7) . . ? C12 C17 C16 131.4(6) . . ? N2 C21 C22 178.1(11) . . ? C21 C22 C27 113.1(8) . . ? C21 C22 C23 122.5(8) . . ? C27 C22 C23 124.4(7) . . ? C24 C23 C22 121.3(8) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 114.2(9) . . ? C23 C24 H24A 122.9 . . ? C25 C24 H24A 122.9 . . ? C24 C25 C26 126.2(8) . . ? C24 C25 H25A 116.9 . . ? C26 C25 H25A 116.9 . . ? C27 C26 C25 118.6(8) . . ? C27 C26 H26A 120.7 . . ? C25 C26 H26A 120.7 . . ? C26 C27 C22 115.3(8) . . ? C26 C27 O1 120.9(7) . . ? C22 C27 O1 123.6(7) . . ? N3 C31 C32 178.2(10) . . ? C31 C32 C33 117.4(7) . . ? C31 C32 C37 119.2(7) . . ? C33 C32 C37 123.2(7) . . ? C34 C33 C32 115.1(7) . . ? C34 C33 H33A 122.5 . . ? C32 C33 H33A 122.5 . . ? C33 C34 C35 119.8(7) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 126.1(7) . . ? C36 C35 H35A 117.0 . . ? C34 C35 H35A 117.0 . . ? C37 C36 C35 113.4(8) . . ? C37 C36 H36A 123.3 . . ? C35 C36 H36A 123.3 . . ? C36 C37 O2 119.8(8) . . ? C36 C37 C32 122.2(7) . . ? O2 C37 C32 117.9(7) . . ? N4 C41 C42 177.5(9) . . ? C43 C42 C41 117.7(10) . . ? C43 C42 C47 112.4(9) . . ? C41 C42 C47 129.4(8) . . ? C42 C43 C44 120.3(12) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C43 C44 C45 124.6(12) . . ? C43 C44 H44A 117.7 . . ? C45 C44 H44A 117.7 . . ? C46 C45 C44 116.1(11) . . ? C46 C45 H45A 121.9 . . ? C44 C45 H45A 121.9 . . ? C45 C46 C47 118.7(12) . . ? C45 C46 H46A 120.7 . . ? C47 C46 H46A 120.7 . . ? O2 C47 C46 116.7(9) . . ? O2 C47 C42 115.4(8) . . ? C46 C47 C42 127.8(9) . . ? N5 C51 C52 175.6(10) . . ? C51 C52 C53 116.8(7) . . ? C51 C52 C57 117.9(7) . . ? C53 C52 C57 125.2(7) . . ? C54 C53 C52 116.2(9) . . ? C54 C53 H53A 121.9 . . ? C52 C53 H53A 121.9 . . ? C53 C54 C55 118.6(9) . . ? C53 C54 H54A 120.7 . . ? C55 C54 H54A 120.7 . . ? C56 C55 C54 124.0(8) . . ? C56 C55 H55A 118.0 . . ? C54 C55 H55A 118.0 . . ? C57 C56 C55 118.7(8) . . ? C57 C56 H56A 120.6 . . ? C55 C56 H56A 120.6 . . ? C56 C57 O3 123.5(8) . . ? C56 C57 C52 117.2(8) . . ? O3 C57 C52 119.3(6) . . ? N6 C61 C62 178.1(10) . . ? C63 C62 C61 115.1(8) . . ? C63 C62 C67 121.9(7) . . ? C61 C62 C67 123.0(7) . . ? C62 C63 C64 114.1(9) . . ? C62 C63 H63A 122.9 . . ? C64 C63 H63A 122.9 . . ? C63 C64 C65 124.1(9) . . ? C63 C64 H64A 117.9 . . ? C65 C64 H64A 117.9 . . ? C66 C65 C64 122.9(9) . . ? C66 C65 H65A 118.6 . . ? C64 C65 H65A 118.6 . . ? C65 C66 C67 114.8(9) . . ? C65 C66 H66A 122.6 . . ? C67 C66 H66A 122.6 . . ? O3 C67 C66 116.6(7) . . ? O3 C67 C62 121.0(7) . . ? C66 C67 C62 122.1(7) . . ? N7 C71 C72 177.2(8) . . ? C71 C72 C73 120.3(8) . . ? C71 C72 C77 121.3(7) . . ? C73 C72 C77 118.4(8) . . ? C74 C73 C72 117.6(10) . . ? C74 C73 H73A 121.2 . . ? C72 C73 H73A 121.2 . . ? C75 C74 C73 123.1(10) . . ? C75 C74 H74A 118.4 . . ? C73 C74 H74A 118.4 . . ? C76 C75 C74 118.2(11) . . ? C76 C75 H75A 120.9 . . ? C74 C75 H75A 120.9 . . ? C77 C76 C75 122.1(12) . . ? C77 C76 H76A 118.9 . . ? C75 C76 H76A 118.9 . . ? C76 C77 O4 125.5(8) . . ? C76 C77 C72 120.4(8) . . ? O4 C77 C72 114.0(7) . . ? N8 C81 C82 179.1(7) . . ? C87 C82 C81 129.4(7) . . ? C87 C82 C83 105.3(7) . . ? C81 C82 C83 125.3(7) . . ? C82 C83 C84 126.8(8) . . ? C82 C83 H83A 116.6 . . ? C84 C83 H83A 116.6 . . ? C85 C84 C83 123.1(10) . . ? C85 C84 H84A 118.4 . . ? C83 C84 H84A 118.4 . . ? C86 C85 C84 113.6(10) . . ? C86 C85 H85A 123.2 . . ? C84 C85 H85A 123.2 . . ? C85 C86 C87 123.7(8) . . ? C85 C86 H86A 118.2 . . ? C87 C86 H86A 118.2 . . ? O4 C87 C82 103.7(7) . . ? O4 C87 C86 128.8(7) . . ? C82 C87 C86 127.5(7) . . ? O6 S1 O8 98.4(5) . . ? O6 S1 O7 141.4(5) . . ? O8 S1 O7 93.5(6) . . ? O6 S1 C1 97.9(5) . . ? O8 S1 C1 102.5(6) . . ? O7 S1 C1 115.2(4) . . ? F2 C1 F3 125.1(7) . . ? F2 C1 F1 94.1(8) . . ? F3 C1 F1 101.3(8) . . ? F2 C1 S1 101.9(5) . . ? F3 C1 S1 125.5(6) . . ? F1 C1 S1 101.1(7) . . ? F2 C1 F10 88.0(7) . . ? F3 C1 F10 77.9(8) . . ? F1 C1 F10 177.8(9) . . ? S1 C1 F10 77.9(6) . . ? O8 F10 C1 90.8(7) . . ? S1 O6 Ag1 126.8(5) . . ? S1 O8 F10 87.3(6) . . ? S2 O9 Ag3 158.4(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.507 _refine_diff_density_min -1.573 _refine_diff_density_rms 0.167 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 286 108 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 895070'