#! data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address K.Fromm ;Departement de Chimie Chemin du Mus\'ee 9 1700 Fribourg Switzerland ; F.Gschwind ;Departement de Chimie Chemin du Mus\'ee 7 1700 Fribourg Switzerland Currently: Max-Planck-Institute for solid state chemistry Heisenbergstrasse 1 70569 Stuttgart ; _publ_contact_author_address ;Departement de Chimie Chemin du Mus\'ee 7 1700 Fribourg Switzerland ; _publ_contact_author_email Katharina.Fromm@unifr.ch _publ_contact_author_phone '+41 26 300 8732' _publ_contact_author_name 'Katharina Fromm' data_h:\20x _database_code_depnum_ccdc_archive 'CCDC 814120' #TrackingRef '4358_web_deposit_cif_file_0_FabienneGschwind_1298368545.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common 'nictotinic acid monoethylene glycol monomethyl ether silver nitrate' _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Ag N2 O6, N O3' _chemical_formula_sum 'C18 H22 Ag N3 O9' _chemical_formula_weight 532.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.977 _cell_length_b 8.818 _cell_length_c 15.252 _cell_angle_alpha 88.62 _cell_angle_beta 79.86 _cell_angle_gamma 76.96 _cell_volume 1028.7 _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4628 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17071 _diffrn_reflns_av_R_equivalents 0.1973 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.33 _reflns_number_total 4633 _reflns_number_gt 3182 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material Word _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^)+(0.1600P)^2^+92.3819P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4633 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1905 _refine_ls_R_factor_gt 0.1445 _refine_ls_wR_factor_ref 0.4215 _refine_ls_wR_factor_gt 0.3917 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.004 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 0.7253(2) 0.07378(17) 0.06486(10) 0.0263(4) Uani 1 1 d . . . C1 C 0.5670(18) 0.308(2) -0.0639(10) 0.016(3) Uani 1 1 d . . . H1 H 0.4805 0.2480 -0.0522 0.019 Uiso 1 1 calc R . . C2 C 0.843(2) 0.344(2) -0.0524(12) 0.023(4) Uani 1 1 d . . . H2 H 0.9513 0.3051 -0.0329 0.028 Uiso 1 1 calc R . . C3 C 0.825(2) 0.478(2) -0.1045(13) 0.029(4) Uani 1 1 d . . . H3 H 0.9137 0.5351 -0.1160 0.035 Uiso 1 1 calc R . . C4 C 0.671(2) 0.524(2) -0.1385(12) 0.026(4) Uani 1 1 d . . . H4 H 0.6559 0.6128 -0.1750 0.031 Uiso 1 1 calc R . . C5 C 0.540(2) 0.442(2) -0.1206(11) 0.022(3) Uani 1 1 d . . . C6 C 0.369(2) 0.487(2) -0.1499(12) 0.025(4) Uani 1 1 d . . . C7 C 0.214(2) 0.654(3) -0.2474(12) 0.030(4) Uani 1 1 d . . . H7A H 0.1319 0.7254 -0.2018 0.036 Uiso 1 1 calc R . . H7B H 0.1591 0.5685 -0.2590 0.036 Uiso 1 1 calc R . . C8 C 0.252(2) 0.740(2) -0.3301(14) 0.029(4) Uani 1 1 d . . . H8A H 0.1405 0.7964 -0.3473 0.035 Uiso 1 1 calc R . . H8B H 0.3192 0.8170 -0.3200 0.035 Uiso 1 1 calc R . . C9 C 0.373(3) 0.717(3) -0.4797(15) 0.041(5) Uani 1 1 d . . . H9A H 0.4400 0.6439 -0.5275 0.061 Uiso 1 1 calc R . . H9B H 0.4370 0.7968 -0.4723 0.061 Uiso 1 1 calc R . . H9C H 0.2591 0.7660 -0.4951 0.061 Uiso 1 1 calc R . . C10 C 0.862(2) -0.1179(18) 0.2182(12) 0.021(3) Uani 1 1 d . . . H10 H 0.9686 -0.0930 0.1900 0.025 Uiso 1 1 calc R . . C11 C 0.566(3) -0.092(2) 0.2276(13) 0.029(4) Uani 1 1 d . . . H11 H 0.4627 -0.0497 0.2043 0.035 Uiso 1 1 calc R . . C12 C 0.558(3) -0.192(3) 0.3014(15) 0.036(5) Uani 1 1 d . . . H12 H 0.4497 -0.2103 0.3311 0.043 Uiso 1 1 calc R . . C13 C 0.712(2) -0.261(2) 0.3290(13) 0.029(4) Uani 1 1 d . . . H13 H 0.7111 -0.3362 0.3748 0.035 Uiso 1 1 calc R . . C14 C 0.865(2) -0.224(2) 0.2915(13) 0.025(4) Uani 1 1 d . . . C15 C 1.035(2) -0.288(2) 0.3209(13) 0.027(4) Uani 1 1 d . . . C16 C 1.203(3) -0.505(3) 0.3810(17) 0.042(5) Uani 1 1 d . . . H16A H 1.3023 -0.4716 0.3428 0.051 Uiso 1 1 calc R . . H16B H 1.1984 -0.4716 0.4431 0.051 Uiso 1 1 calc R . . C17 C 1.228(3) -0.678(3) 0.3753(16) 0.039(5) Uani 1 1 d . . . H17A H 1.1896 -0.7063 0.3210 0.047 Uiso 1 1 calc R . . H17B H 1.3538 -0.7276 0.3710 0.047 Uiso 1 1 calc R . . C18 C 1.172(3) -0.895(3) 0.457(2) 0.050(6) Uani 1 1 d . . . H18A H 1.1069 -0.9290 0.5121 0.076 Uiso 1 1 calc R . . H18B H 1.2978 -0.9303 0.4573 0.076 Uiso 1 1 calc R . . H18C H 1.1426 -0.9403 0.4056 0.076 Uiso 1 1 calc R . . N1 N 0.710(2) 0.2666(16) -0.0282(11) 0.028(3) Uani 1 1 d . . . N2 N 0.718(2) -0.0545(15) 0.1895(10) 0.023(3) Uani 1 1 d . . . N3 N 0.207(2) 0.1105(17) 0.1103(10) 0.026(3) Uani 1 1 d . . . O1 O 0.2430(17) 0.4359(16) -0.1224(9) 0.030(3) Uani 1 1 d . . . O2 O 0.3740(16) 0.5929(16) -0.2157(10) 0.030(3) Uani 1 1 d . . . O3 O 0.3482(17) 0.6357(15) -0.4000(9) 0.030(3) Uani 1 1 d . . . O4 O 1.1498(18) -0.2159(17) 0.3185(12) 0.043(4) Uani 1 1 d . . . O5 O 1.0389(17) -0.4342(16) 0.3506(10) 0.031(3) Uani 1 1 d . . . O6 O 1.129(2) -0.7351(17) 0.4534(10) 0.039(3) Uani 1 1 d . . . O7 O 0.1822(19) 0.1418(16) 0.1921(10) 0.037(3) Uani 1 1 d . . . O8 O 0.3653(19) 0.075(2) 0.0657(8) 0.044(4) Uani 1 1 d . . . O9 O 0.0630(16) 0.1162(15) 0.0717(7) 0.023(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 0.0294(7) 0.0247(7) 0.0238(7) 0.0044(5) -0.0084(5) -0.0021(5) C1 0.006(6) 0.033(9) 0.009(6) -0.003(6) 0.002(5) -0.007(6) C2 0.019(8) 0.026(8) 0.029(9) -0.009(7) -0.019(7) -0.001(6) C3 0.015(8) 0.046(11) 0.028(9) 0.012(8) -0.007(7) -0.009(7) C4 0.030(9) 0.025(8) 0.024(9) -0.004(7) -0.014(7) -0.002(7) C5 0.008(7) 0.034(9) 0.022(8) 0.009(7) 0.000(6) -0.002(6) C6 0.011(7) 0.038(10) 0.024(9) -0.013(7) 0.001(6) -0.002(7) C7 0.020(8) 0.051(12) 0.018(8) 0.004(8) -0.014(7) 0.004(8) C8 0.025(9) 0.017(8) 0.045(11) 0.009(7) -0.021(8) 0.005(7) C9 0.058(14) 0.038(11) 0.034(11) 0.016(9) -0.020(10) -0.020(10) C10 0.027(8) 0.011(7) 0.024(8) 0.004(6) -0.007(7) 0.000(6) C11 0.035(10) 0.026(9) 0.028(9) 0.007(7) -0.016(8) -0.002(8) C12 0.024(9) 0.042(11) 0.045(12) 0.006(9) -0.001(8) -0.021(8) C13 0.029(9) 0.020(8) 0.030(10) 0.009(7) -0.004(8) 0.008(7) C14 0.015(8) 0.027(9) 0.032(10) 0.005(7) -0.007(7) -0.002(7) C15 0.023(9) 0.027(9) 0.030(10) 0.006(7) -0.001(7) -0.003(7) C16 0.047(13) 0.040(12) 0.044(13) 0.012(10) -0.014(11) -0.017(10) C17 0.035(11) 0.037(11) 0.045(12) 0.006(9) -0.014(10) -0.002(9) C18 0.043(13) 0.031(11) 0.077(18) 0.011(11) -0.023(13) 0.000(9) N1 0.036(9) 0.014(7) 0.037(9) 0.004(6) -0.016(7) -0.007(6) N2 0.033(8) 0.009(6) 0.025(7) 0.002(5) -0.005(6) -0.001(6) N3 0.038(9) 0.020(7) 0.026(8) 0.008(6) -0.018(7) -0.010(6) O1 0.028(7) 0.036(7) 0.026(7) 0.008(5) -0.009(5) -0.005(6) O2 0.018(6) 0.034(7) 0.042(8) 0.015(6) -0.020(6) 0.000(5) O3 0.026(7) 0.029(7) 0.031(7) 0.007(5) 0.001(5) -0.005(5) O4 0.023(7) 0.035(8) 0.078(12) 0.016(8) -0.029(7) -0.008(6) O5 0.022(6) 0.031(7) 0.040(8) 0.005(6) -0.006(6) -0.008(5) O6 0.051(9) 0.030(7) 0.033(8) 0.006(6) -0.005(7) -0.011(6) O7 0.033(7) 0.026(7) 0.047(9) -0.013(6) -0.008(7) 0.005(6) O8 0.036(8) 0.103(13) 0.006(5) -0.009(7) 0.006(5) -0.051(9) O9 0.026(6) 0.036(7) 0.011(5) -0.016(5) 0.011(5) -0.023(5) _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 2.184(15) . ? Ag1 N2 2.187(15) . ? C1 N1 1.32(2) . ? C1 C5 1.45(2) . ? C1 H1 0.9500 . ? C2 N1 1.38(2) . ? C2 C3 1.40(3) . ? C2 H2 0.9500 . ? C3 C4 1.39(2) . ? C3 H3 0.9500 . ? C4 C5 1.38(3) . ? C4 H4 0.9500 . ? C5 C6 1.47(2) . ? C6 O1 1.20(2) . ? C6 O2 1.36(2) . ? C7 O2 1.430(19) . ? C7 C8 1.47(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.42(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O3 1.40(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.31(2) . ? C10 C14 1.44(2) . ? C10 H10 0.9500 . ? C11 N2 1.35(3) . ? C11 C12 1.42(3) . ? C11 H11 0.9500 . ? C12 C13 1.37(3) . ? C12 H12 0.9500 . ? C13 C14 1.36(3) . ? C13 H13 0.9500 . ? C14 C15 1.49(2) . ? C15 O4 1.23(2) . ? C15 O5 1.35(2) . ? C16 C17 1.50(3) . ? C16 O5 1.47(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O6 1.46(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O6 1.38(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N3 O7 1.26(2) . ? N3 O9 1.368(19) . ? N3 O8 1.30(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 160.9(5) . . ? N1 C1 C5 121.4(15) . . ? N1 C1 H1 119.3 . . ? C5 C1 H1 119.3 . . ? N1 C2 C3 122.5(15) . . ? N1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C4 C3 C2 117.3(17) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C5 C4 C3 121.6(18) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C1 117.6(15) . . ? C4 C5 C6 125.2(16) . . ? C1 C5 C6 117.0(15) . . ? O1 C6 O2 123.5(16) . . ? O1 C6 C5 126.0(18) . . ? O2 C6 C5 110.5(15) . . ? O2 C7 C8 109.1(16) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O3 C8 C7 110.6(15) . . ? O3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C14 121.8(16) . . ? N2 C10 H10 119.1 . . ? C14 C10 H10 119.1 . . ? N2 C11 C12 121.4(17) . . ? N2 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 118.1(18) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C14 C13 C12 120.8(17) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C10 117.9(16) . . ? C13 C14 C15 124.0(17) . . ? C10 C14 C15 118.0(16) . . ? O4 C15 O5 126.6(17) . . ? O4 C15 C14 124.0(17) . . ? O5 C15 C14 109.4(16) . . ? C17 C16 O5 107.8(18) . . ? C17 C16 H16A 110.2 . . ? O5 C16 H16A 110.2 . . ? C17 C16 H16B 110.2 . . ? O5 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O6 C17 C16 110.8(19) . . ? O6 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 N1 C2 119.2(15) . . ? C1 N1 Ag1 117.8(12) . . ? C2 N1 Ag1 123.0(12) . . ? C10 N2 C11 119.7(15) . . ? C10 N2 Ag1 120.5(12) . . ? C11 N2 Ag1 118.7(12) . . ? O7 N3 O9 117.9(15) . . ? O7 N3 O8 119.4(15) . . ? O9 N3 O8 122.7(14) . . ? C6 O2 C7 116.8(15) . . ? C9 O3 C8 110.1(15) . . ? C15 O5 C16 112.4(15) . . ? C18 O6 C17 111.8(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -6(3) . . . . ? C2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C1 1(3) . . . . ? C3 C4 C5 C6 176.6(17) . . . . ? N1 C1 C5 C4 2(2) . . . . ? N1 C1 C5 C6 -174.3(15) . . . . ? C4 C5 C6 O1 -165.8(19) . . . . ? C1 C5 C6 O1 10(3) . . . . ? C4 C5 C6 O2 16(3) . . . . ? C1 C5 C6 O2 -167.7(15) . . . . ? O2 C7 C8 O3 68(2) . . . . ? N2 C11 C12 C13 -5(3) . . . . ? C11 C12 C13 C14 6(3) . . . . ? C12 C13 C14 C10 -4(3) . . . . ? C12 C13 C14 C15 176.7(19) . . . . ? N2 C10 C14 C13 2(3) . . . . ? N2 C10 C14 C15 -178.8(16) . . . . ? C13 C14 C15 O4 -147(2) . . . . ? C10 C14 C15 O4 33(3) . . . . ? C13 C14 C15 O5 32(3) . . . . ? C10 C14 C15 O5 -147.2(17) . . . . ? O5 C16 C17 O6 -82(2) . . . . ? C5 C1 N1 C2 -6(2) . . . . ? C5 C1 N1 Ag1 174.9(12) . . . . ? C3 C2 N1 C1 8(3) . . . . ? C3 C2 N1 Ag1 -173.0(14) . . . . ? N2 Ag1 N1 C1 -101(2) . . . . ? N2 Ag1 N1 C2 80(2) . . . . ? C14 C10 N2 C11 -2(3) . . . . ? C14 C10 N2 Ag1 -169.5(13) . . . . ? C12 C11 N2 C10 3(3) . . . . ? C12 C11 N2 Ag1 171.5(15) . . . . ? N1 Ag1 N2 C10 -101(2) . . . . ? N1 Ag1 N2 C11 91(2) . . . . ? O1 C6 O2 C7 6(3) . . . . ? C5 C6 O2 C7 -176.4(15) . . . . ? C8 C7 O2 C6 -168.0(16) . . . . ? C7 C8 O3 C9 176.0(16) . . . . ? O4 C15 O5 C16 -1(3) . . . . ? C14 C15 O5 C16 -179.9(17) . . . . ? C17 C16 O5 C15 -156.4(18) . . . . ? C16 C17 O6 C18 -169.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.830 _refine_diff_density_min -2.158 _refine_diff_density_rms 0.310 # Attachment '4359_web_deposit_cif_file_1_FabienneGschwind_1298368545.cif' data_4577 _database_code_depnum_ccdc_archive 'CCDC 814121' _audit_creation_method shelxl-97 _chemical_name_systematic ? _chemical_name_common 'Triethylene glycol monomethyl ether nicotinate silver hexafluorophosphat' _chemical_formula_moiety 'C26 H38 Ag N2 O10, F6 P' _chemical_formula_sum 'C26 H38 Ag F6 N2 O10 P' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour colourless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 791.42 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' 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' f f 0.0171 0.0103 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.512(3) _cell_length_b 14.026(3) _cell_length_c 18.400(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.63(3) _cell_angle_gamma 90.00 _cell_volume 3229.1(11) _cell_formula_units_z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3403 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.73 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 1616 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_t_min 0.8614 _exptl_absorpt_correction_t_max 0.8619 _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22976 _diffrn_reflns_av_r_equivalents 0.0932 _diffrn_reflns_av_sigmai/neti 0.0403 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3403 _reflns_number_gt 2850 _reflns_threshold_expression >2sigma(i) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material Word _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^)+(0.0457p)^2^+7.3436p] 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 3403 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0563 _refine_ls_r_factor_gt 0.0440 _refine_ls_wr_factor_ref 0.1095 _refine_ls_wr_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_s_all 1.079 _refine_ls_shift/su_max 0.005 _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 c1 c 0.5814(2) 0.0762(2) 0.64540(16) 0.0335(6) uani 1 1 d . . . h1 h 0.5926 0.0100 0.6532 0.040 uiso 1 1 calc r . . c2 c 0.5206(3) 0.1988(2) 0.57250(19) 0.0417(7) uani 1 1 d . . . h2 h 0.4875 0.2194 0.5285 0.050 uiso 1 1 calc r . . c3 c 0.5509(3) 0.2663(2) 0.6231(2) 0.0479(9) uani 1 1 d . . . h3 h 0.5394 0.3321 0.6137 0.057 uiso 1 1 calc r . . c4 c 0.5981(3) 0.2374(2) 0.68728(19) 0.0429(8) uani 1 1 d . . . h4 h 0.6202 0.2829 0.7226 0.052 uiso 1 1 calc r . . c5 c 0.6128(2) 0.1404(2) 0.69949(17) 0.0349(7) uani 1 1 d . . . c6 c 0.6581(2) 0.1084(3) 0.77070(18) 0.0396(7) uani 1 1 d . . . c7 c 0.7017(3) -0.0223(3) 0.8457(2) 0.0507(9) uani 1 1 d . . . h7a h 0.6739 0.0171 0.8860 0.061 uiso 1 1 calc r . . h7b h 0.7807 -0.0201 0.8475 0.061 uiso 1 1 calc r . . c8 c 0.6638(3) -0.1227(3) 0.8530(2) 0.0520(9) uani 1 1 d . . . h8a h 0.6814 -0.1594 0.8088 0.062 uiso 1 1 calc r . . h8b h 0.6993 -0.1536 0.8952 0.062 uiso 1 1 calc r . . c9 c 0.5050(4) -0.2126(2) 0.8629(2) 0.0525(10) uani 1 1 d . . . h9a h 0.5290 -0.2484 0.9065 0.063 uiso 1 1 calc r . . h9b h 0.5271 -0.2484 0.8193 0.063 uiso 1 1 calc r . . c10 c 0.3887(4) -0.2020(3) 0.8632(2) 0.0611(11) uani 1 1 d . . . h10a h 0.3655 -0.1641 0.8204 0.073 uiso 1 1 calc r . . h10b h 0.3547 -0.2656 0.8598 0.073 uiso 1 1 calc r . . c11 c 0.2420(4) -0.1395(4) 0.9224(4) 0.0897(17) uani 1 1 d . . . h11a h 0.2250 -0.1040 0.8772 0.108 uiso 1 1 calc r . . h11b h 0.2037 -0.2012 0.9207 0.108 uiso 1 1 calc r . . c12 c 0.2083(4) -0.0861(4) 0.9837(4) 0.0925(19) uani 1 1 d . . . h12a h 0.2319 -0.1200 1.0282 0.111 uiso 1 1 calc r . . h12b h 0.1292 -0.0846 0.9836 0.111 uiso 1 1 calc r . . c13 c 0.1846(4) 0.0812(4) 0.9517(3) 0.0745(14) uani 1 1 d . . . h13a h 0.2197 0.1434 0.9572 0.112 uiso 1 1 calc r . . h13b h 0.1134 0.0838 0.9733 0.112 uiso 1 1 calc r . . h13c h 0.1779 0.0655 0.9000 0.112 uiso 1 1 calc r . . n1 n 0.5360(2) 0.10463(18) 0.58294(13) 0.0352(6) uani 1 1 d . . . o1 o 0.66249(19) 0.01385(17) 0.77624(12) 0.0433(5) uani 1 1 d . . . o2 o 0.6836(2) 0.1632(2) 0.81801(14) 0.0542(7) uani 1 1 d . . . o3 o 0.55196(19) -0.12111(16) 0.86283(13) 0.0446(6) uani 1 1 d . . . o4 o 0.3559(2) -0.15606(19) 0.92741(18) 0.0613(7) uani 1 1 d . . . o5 o 0.2468(2) 0.01037(19) 0.98755(17) 0.0592(7) uani 1 1 d . . . ag1 ag 0.5000 0.0000 0.5000 0.04357(14) uani 1 2 d s . . f2 f 0.91101(19) -0.05842(15) 0.73769(13) 0.0605(6) uani 1 1 d . . . f3 f 0.91103(18) 0.10113(14) 0.73774(13) 0.0576(6) uani 1 1 d . . . f1 f 1.0242(2) 0.02143(19) 0.66480(12) 0.0634(6) uani 1 1 d . . . p1 p 1.0000 0.02167(7) 0.7500 0.0356(3) uani 1 2 d s . . loop_ _atom_site_aniso_label _atom_site_aniso_u_11 _atom_site_aniso_u_22 _atom_site_aniso_u_33 _atom_site_aniso_u_23 _atom_site_aniso_u_13 _atom_site_aniso_u_12 c1 0.0347(16) 0.0299(14) 0.0359(15) -0.0078(12) 0.0026(12) -0.0032(12) c2 0.052(2) 0.0331(16) 0.0395(17) 0.0011(13) 0.0068(15) 0.0009(14) c3 0.063(2) 0.0268(15) 0.054(2) -0.0052(14) 0.0129(17) -0.0069(15) c4 0.0454(19) 0.0361(17) 0.0475(19) -0.0147(14) 0.0101(15) -0.0136(14) c5 0.0311(16) 0.0364(16) 0.0373(16) -0.0104(13) 0.0042(12) -0.0072(12) c6 0.0277(15) 0.053(2) 0.0387(17) -0.0136(14) 0.0027(13) -0.0047(14) c7 0.0349(18) 0.077(3) 0.0397(18) 0.0022(17) -0.0084(14) 0.0026(17) c8 0.047(2) 0.067(2) 0.0418(19) -0.0006(17) -0.0043(16) 0.0224(18) c9 0.083(3) 0.0305(16) 0.044(2) -0.0062(14) -0.0005(19) 0.0016(17) c10 0.084(3) 0.045(2) 0.055(2) -0.0079(17) -0.009(2) -0.022(2) c11 0.064(3) 0.082(4) 0.123(5) -0.031(3) 0.001(3) -0.027(3) c12 0.065(3) 0.090(4) 0.122(5) -0.042(3) 0.022(3) -0.033(3) c13 0.059(3) 0.105(4) 0.059(3) 0.000(3) -0.008(2) 0.018(3) n1 0.0427(15) 0.0313(13) 0.0318(13) -0.0061(10) 0.0028(11) -0.0043(11) o1 0.0415(13) 0.0540(15) 0.0344(11) -0.0043(10) -0.0055(9) 0.0011(10) o2 0.0460(15) 0.0693(17) 0.0470(14) -0.0234(12) -0.0080(11) -0.0078(12) o3 0.0495(14) 0.0318(11) 0.0524(14) -0.0042(10) -0.0082(11) 0.0068(10) o4 0.0492(16) 0.0496(15) 0.085(2) -0.0101(14) 0.0020(14) -0.0104(12) o5 0.0534(16) 0.0553(16) 0.0689(18) -0.0100(13) -0.0064(13) -0.0063(13) ag1 0.0587(3) 0.0402(2) 0.03180(19) -0.01372(14) 0.00121(14) -0.00584(17) f2 0.0683(15) 0.0342(11) 0.0785(16) 0.0014(10) -0.0164(12) -0.0149(10) f3 0.0521(13) 0.0366(11) 0.0842(16) 0.0054(10) 0.0104(11) 0.0128(9) f1 0.0641(15) 0.0817(17) 0.0445(12) 0.0032(11) 0.0053(10) 0.0158(12) p1 0.0426(6) 0.0209(5) 0.0432(6) 0.000 0.0013(5) 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 c1 n1 1.337(4) . ? c1 c5 1.395(4) . ? c1 h1 0.9500 . ? c2 n1 1.348(4) . ? c2 c3 1.378(5) . ? c2 h2 0.9500 . ? c3 c4 1.376(5) . ? c3 h3 0.9500 . ? c4 c5 1.391(5) . ? c4 h4 0.9500 . ? c5 c6 1.491(5) . ? c6 o2 1.202(4) . ? c6 o1 1.331(4) . ? c7 o1 1.456(4) . ? c7 c8 1.492(6) . ? c7 h7a 0.9900 . ? c7 h7b 0.9900 . ? c8 o3 1.413(4) . ? c8 h8a 0.9900 . ? c8 h8b 0.9900 . ? c9 o3 1.411(4) . ? c9 c10 1.463(6) . ? c9 h9a 0.9900 . ? c9 h9b 0.9900 . ? c10 o4 1.411(5) . ? c10 h10a 0.9900 . ? c10 h10b 0.9900 . ? c11 c12 1.422(8) . ? c11 o4 1.445(6) . ? c11 h11a 0.9900 . ? c11 h11b 0.9900 . ? c12 o5 1.437(6) . ? c12 h12a 0.9900 . ? c12 h12b 0.9900 . ? c13 o5 1.420(5) . ? c13 h13a 0.9800 . ? c13 h13b 0.9800 . ? c13 h13c 0.9800 . ? n1 ag1 2.161(2) . ? ag1 n1 2.161(2) 5_656 ? f2 p1 1.596(2) . ? f3 p1 1.590(2) . ? f1 p1 1.600(2) . ? p1 f3 1.590(2) 2_756 ? p1 f2 1.596(2) 2_756 ? p1 f1 1.600(2) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag n1 c1 c5 122.3(3) . . ? n1 c1 h1 118.8 . . ? c5 c1 h1 118.8 . . ? n1 c2 c3 122.6(3) . . ? n1 c2 h2 118.7 . . ? c3 c2 h2 118.7 . . ? c4 c3 c2 119.3(3) . . ? c4 c3 h3 120.3 . . ? c2 c3 h3 120.3 . . ? c3 c4 c5 118.8(3) . . ? c3 c4 h4 120.6 . . ? c5 c4 h4 120.6 . . ? c4 c5 c1 118.7(3) . . ? c4 c5 c6 119.0(3) . . ? c1 c5 c6 122.3(3) . . ? o2 c6 o1 124.9(3) . . ? o2 c6 c5 122.6(3) . . ? o1 c6 c5 112.5(3) . . ? o1 c7 c8 107.7(3) . . ? o1 c7 h7a 110.2 . . ? c8 c7 h7a 110.2 . . ? o1 c7 h7b 110.2 . . ? c8 c7 h7b 110.2 . . ? h7a c7 h7b 108.5 . . ? o3 c8 c7 108.2(3) . . ? o3 c8 h8a 110.1 . . ? c7 c8 h8a 110.1 . . ? o3 c8 h8b 110.1 . . ? c7 c8 h8b 110.1 . . ? h8a c8 h8b 108.4 . . ? o3 c9 c10 108.8(3) . . ? o3 c9 h9a 109.9 . . ? c10 c9 h9a 109.9 . . ? o3 c9 h9b 109.9 . . ? c10 c9 h9b 109.9 . . ? h9a c9 h9b 108.3 . . ? o4 c10 c9 110.4(3) . . ? o4 c10 h10a 109.6 . . ? c9 c10 h10a 109.6 . . ? o4 c10 h10b 109.6 . . ? c9 c10 h10b 109.6 . . ? h10a c10 h10b 108.1 . . ? c12 c11 o4 109.6(4) . . ? c12 c11 h11a 109.8 . . ? o4 c11 h11a 109.8 . . ? c12 c11 h11b 109.8 . . ? o4 c11 h11b 109.8 . . ? h11a c11 h11b 108.2 . . ? c11 c12 o5 115.7(5) . . ? c11 c12 h12a 108.4 . . ? o5 c12 h12a 108.4 . . ? c11 c12 h12b 108.4 . . ? o5 c12 h12b 108.4 . . ? h12a c12 h12b 107.4 . . ? o5 c13 h13a 109.5 . . ? o5 c13 h13b 109.5 . . ? h13a c13 h13b 109.5 . . ? o5 c13 h13c 109.5 . . ? h13a c13 h13c 109.5 . . ? h13b c13 h13c 109.5 . . ? c1 n1 c2 118.2(3) . . ? c1 n1 ag1 119.2(2) . . ? c2 n1 ag1 122.4(2) . . ? c6 o1 c7 115.3(3) . . ? c9 o3 c8 113.5(3) . . ? c10 o4 c11 108.4(4) . . ? c13 o5 c12 117.1(4) . . ? n1 ag1 n1 180.0 5_656 . ? f3 p1 f3 90.96(17) 2_756 . ? f3 p1 f2 179.78(14) 2_756 . ? f3 p1 f2 89.26(12) . . ? f3 p1 f2 89.26(12) 2_756 2_756 ? f3 p1 f2 179.78(14) . 2_756 ? f2 p1 f2 90.53(18) . 2_756 ? f3 p1 f1 90.05(14) 2_756 . ? f3 p1 f1 90.12(13) . . ? f2 p1 f1 89.92(14) . . ? f2 p1 f1 89.91(13) 2_756 . ? f3 p1 f1 90.12(13) 2_756 2_756 ? f3 p1 f1 90.05(14) . 2_756 ? f2 p1 f1 89.91(13) . 2_756 ? f2 p1 f1 89.92(14) 2_756 2_756 ? f1 p1 f1 179.8(2) . 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag n1 c2 c3 c4 -0.6(6) . . . . ? c2 c3 c4 c5 -0.6(5) . . . . ? c3 c4 c5 c1 1.5(5) . . . . ? c3 c4 c5 c6 -176.5(3) . . . . ? n1 c1 c5 c4 -1.2(5) . . . . ? n1 c1 c5 c6 176.7(3) . . . . ? c4 c5 c6 o2 -0.7(5) . . . . ? c1 c5 c6 o2 -178.7(3) . . . . ? c4 c5 c6 o1 176.7(3) . . . . ? c1 c5 c6 o1 -1.2(4) . . . . ? o1 c7 c8 o3 -69.8(4) . . . . ? o3 c9 c10 o4 -63.1(4) . . . . ? o4 c11 c12 o5 67.5(7) . . . . ? c5 c1 n1 c2 0.0(5) . . . . ? c5 c1 n1 ag1 176.0(2) . . . . ? c3 c2 n1 c1 0.9(5) . . . . ? c3 c2 n1 ag1 -174.9(3) . . . . ? o2 c6 o1 c7 0.0(5) . . . . ? c5 c6 o1 c7 -177.4(3) . . . . ? c8 c7 o1 c6 159.0(3) . . . . ? c10 c9 o3 c8 -172.2(3) . . . . ? c7 c8 o3 c9 173.8(3) . . . . ? c9 c10 o4 c11 174.9(4) . . . . ? c12 c11 o4 c10 -175.1(5) . . . . ? c11 c12 o5 c13 87.8(6) . . . . ? c1 n1 ag1 n1 112(100) . . . 5_656 ? c2 n1 ag1 n1 -72(100) . . . 5_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.095 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.068 # Attachment '4360_web_deposit_cif_file_2_FabienneGschwind_1298368545.cif' data_24b _database_code_depnum_ccdc_archive 'CCDC 814122' #TrackingRef '4360_web_deposit_cif_file_2_FabienneGschwind_1298368545.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'monoethylene glycol monomethylether silver triflate' _chemical_melting_point ? _chemical_formula_moiety 'C19 H22 Ag F3 N2 O9 S' _chemical_formula_sum 'C19 H22 Ag F3 N2 O9 S' _chemical_formula_weight 619.32 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6012(17) _cell_length_b 9.789(2) _cell_length_c 15.478(3) _cell_angle_alpha 80.60(3) _cell_angle_beta 85.47(3) _cell_angle_gamma 66.02(3) _cell_volume 1174.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4946 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.72 _exptl_crystal_description needle _exptl_crystal_colour white _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type cylinder _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_absorpt_correction_T_min 0.7139 _exptl_absorpt_correction_T_max 0.7161 _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10682 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.72 _reflns_number_total 4946 _reflns_number_gt 4471 _reflns_threshold_expression >2\s(I) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material Word _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^ > 2\s(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^+0.6077P] 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 0.0017(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4946 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.600936(18) 0.584450(17) 0.539124(9) 0.02877(6) Uani 1 1 d . . . C1 C 0.8895(2) 0.5225(2) 0.40439(12) 0.0247(4) Uani 1 1 d . . . H1 H 0.8311 0.6282 0.3874 0.030 Uiso 1 1 calc R . . C10 C 0.3241(2) 0.6588(2) 0.68038(12) 0.0244(4) Uani 1 1 d . . . H10 H 0.3618 0.5519 0.6896 0.029 Uiso 1 1 calc R . . C14 C 0.1941(2) 0.7424(2) 0.73334(12) 0.0243(4) Uani 1 1 d . . . C11 C 0.3446(2) 0.8743(2) 0.60486(12) 0.0281(4) Uani 1 1 d . . . H11 H 0.3985 0.9205 0.5608 0.034 Uiso 1 1 calc R . . C12 C 0.2140(3) 0.9651(2) 0.65423(13) 0.0298(4) Uani 1 1 d . . . H12 H 0.1783 1.0718 0.6437 0.036 Uiso 1 1 calc R . . C13 C 0.1362(2) 0.8992(2) 0.71905(12) 0.0274(4) Uani 1 1 d . . . H13 H 0.0450 0.9595 0.7532 0.033 Uiso 1 1 calc R . . C2 C 0.9106(2) 0.3036(2) 0.49547(12) 0.0274(4) Uani 1 1 d . . . H2 H 0.8690 0.2546 0.5441 0.033 Uiso 1 1 calc R . . C3 C 1.0544(3) 0.2191(2) 0.45158(13) 0.0303(4) Uani 1 1 d . . . H3 H 1.1090 0.1131 0.4689 0.036 Uiso 1 1 calc R . . C4 C 1.1190(2) 0.2894(2) 0.38204(12) 0.0283(4) Uani 1 1 d . . . H4 H 1.2177 0.2326 0.3508 0.034 Uiso 1 1 calc R . . C5 C 1.0366(2) 0.4449(2) 0.35882(12) 0.0257(4) Uani 1 1 d . . . C15 C 0.1304(2) 0.6570(2) 0.80555(12) 0.0283(4) Uani 1 1 d . . . C6 C 1.1004(2) 0.5357(2) 0.28991(12) 0.0287(4) Uani 1 1 d . . . C19 C 0.4628(3) 0.8886(3) 0.24496(15) 0.0403(5) Uani 1 1 d . . . C7 C 1.3085(3) 0.5269(3) 0.17926(14) 0.0353(4) Uani 1 1 d . . . H7A H 1.3569 0.5799 0.2113 0.042 Uiso 1 1 calc R . . H7B H 1.2255 0.6028 0.1366 0.042 Uiso 1 1 calc R . . C8 C 1.4475(3) 0.4124(3) 0.13244(14) 0.0379(5) Uani 1 1 d . . . H8A H 1.5366 0.4504 0.1121 0.046 Uiso 1 1 calc R . . H8B H 1.5003 0.3173 0.1731 0.046 Uiso 1 1 calc R . . C17 C -0.1027(3) 0.7742(3) 1.00227(15) 0.0410(5) Uani 1 1 d . . . H17A H -0.1883 0.8695 0.9725 0.049 Uiso 1 1 calc R . . H17B H -0.1609 0.7308 1.0496 0.049 Uiso 1 1 calc R . . C16 C -0.0213(3) 0.6656(3) 0.93839(14) 0.0415(5) Uani 1 1 d . . . H16A H 0.0781 0.5781 0.9651 0.050 Uiso 1 1 calc R . . H16B H -0.1035 0.6281 0.9210 0.050 Uiso 1 1 calc R . . N2 N 0.39850(19) 0.72255(17) 0.61686(10) 0.0253(3) Uani 1 1 d . . . N1 N 0.82675(19) 0.45384(17) 0.47156(10) 0.0253(3) Uani 1 1 d . . . O8 O 0.5380(2) 0.84765(18) 0.40746(10) 0.0407(4) Uani 1 1 d . . . O5 O 0.03242(19) 0.74567(17) 0.86209(9) 0.0343(3) Uani 1 1 d . . . O9 O 0.44494(19) 0.67112(15) 0.35888(10) 0.0356(3) Uani 1 1 d . . . O2 O 1.22411(18) 0.44802(16) 0.24058(9) 0.0320(3) Uani 1 1 d . . . O1 O 1.0504(2) 0.67067(16) 0.28257(10) 0.0376(3) Uani 1 1 d . . . O4 O 0.1681(2) 0.52324(17) 0.81306(10) 0.0395(3) Uani 1 1 d . . . O7 O 0.24173(19) 0.92589(17) 0.37058(12) 0.0439(4) Uani 1 1 d . . . O3 O 1.38052(19) 0.3845(2) 0.05999(10) 0.0437(4) Uani 1 1 d . . . O6 O 0.02433(19) 0.80261(17) 1.03745(10) 0.0372(3) Uani 1 1 d . . . F1 F 0.3635(3) 0.8729(2) 0.18966(10) 0.0711(5) Uani 1 1 d . . . F2 F 0.6224(2) 0.8109(2) 0.22355(11) 0.0686(5) Uani 1 1 d . . . F3 F 0.4380(2) 1.03378(17) 0.23364(10) 0.0616(4) Uani 1 1 d . . . S1 S 0.41566(6) 0.82724(5) 0.35794(3) 0.02660(10) Uani 1 1 d . . . C18 C -0.0426(4) 0.9069(3) 1.09868(15) 0.0474(6) Uani 1 1 d . . . H18A H -0.1235 1.0035 1.0693 0.071 Uiso 1 1 calc R . . H18B H 0.0505 0.9222 1.1224 0.071 Uiso 1 1 calc R . . H18C H -0.1009 0.8668 1.1465 0.071 Uiso 1 1 calc R . . C9 C 1.5064(3) 0.2683(4) 0.01819(19) 0.0573(7) Uani 1 1 d . . . H9A H 1.6077 0.2908 0.0058 0.086 Uiso 1 1 calc R . . H9B H 1.4617 0.2625 -0.0368 0.086 Uiso 1 1 calc R . . H9C H 1.5366 0.1715 0.0567 0.086 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 Ag1 0.02756(9) 0.02894(9) 0.02832(9) -0.00980(5) 0.00508(5) -0.00863(6) C1 0.0277(9) 0.0224(9) 0.0255(9) -0.0064(7) -0.0008(7) -0.0103(7) C10 0.0280(9) 0.0215(8) 0.0237(9) -0.0049(7) -0.0026(7) -0.0089(7) C14 0.0276(9) 0.0262(9) 0.0214(8) -0.0051(7) -0.0016(7) -0.0122(7) C11 0.0353(10) 0.0246(9) 0.0270(9) -0.0047(7) 0.0023(7) -0.0148(8) C12 0.0394(10) 0.0194(9) 0.0286(9) -0.0051(7) 0.0014(8) -0.0095(8) C13 0.0293(9) 0.0262(9) 0.0260(9) -0.0103(7) 0.0004(7) -0.0081(7) C2 0.0331(9) 0.0256(9) 0.0248(9) -0.0041(7) -0.0020(7) -0.0126(8) C3 0.0360(10) 0.0222(9) 0.0294(10) -0.0044(7) -0.0023(8) -0.0078(8) C4 0.0279(9) 0.0263(9) 0.0272(9) -0.0092(7) 0.0003(7) -0.0055(8) C5 0.0293(9) 0.0258(9) 0.0233(9) -0.0065(7) -0.0022(7) -0.0111(7) C15 0.0323(9) 0.0321(10) 0.0242(9) -0.0063(7) -0.0009(7) -0.0155(8) C6 0.0294(9) 0.0331(10) 0.0253(9) -0.0062(8) -0.0007(7) -0.0133(8) C19 0.0528(13) 0.0355(11) 0.0338(11) -0.0038(9) 0.0018(9) -0.0198(10) C7 0.0350(10) 0.0420(12) 0.0306(10) -0.0026(9) 0.0037(8) -0.0188(9) C8 0.0273(9) 0.0533(13) 0.0318(10) -0.0043(9) 0.0018(8) -0.0158(9) C17 0.0396(11) 0.0516(14) 0.0337(11) -0.0078(10) 0.0109(9) -0.0217(10) C16 0.0567(14) 0.0490(13) 0.0320(11) -0.0080(9) 0.0124(10) -0.0361(12) N2 0.0280(8) 0.0230(8) 0.0253(8) -0.0078(6) 0.0017(6) -0.0093(6) N1 0.0247(7) 0.0249(8) 0.0266(8) -0.0071(6) 0.0000(6) -0.0088(6) O8 0.0540(9) 0.0435(9) 0.0337(8) -0.0031(7) -0.0037(7) -0.0291(8) O5 0.0425(8) 0.0363(8) 0.0276(7) -0.0078(6) 0.0112(6) -0.0202(7) O9 0.0421(8) 0.0188(7) 0.0445(8) -0.0074(6) 0.0062(6) -0.0108(6) O2 0.0330(7) 0.0331(7) 0.0293(7) -0.0059(6) 0.0065(6) -0.0132(6) O1 0.0462(8) 0.0277(8) 0.0388(8) -0.0048(6) 0.0065(6) -0.0159(7) O4 0.0570(9) 0.0315(8) 0.0350(8) -0.0052(6) 0.0063(7) -0.0239(7) O7 0.0355(8) 0.0262(7) 0.0588(10) -0.0075(7) 0.0133(7) -0.0030(6) O3 0.0301(7) 0.0647(11) 0.0354(8) -0.0181(8) 0.0038(6) -0.0149(7) O6 0.0416(8) 0.0360(8) 0.0320(8) -0.0094(6) 0.0056(6) -0.0128(7) F1 0.1057(14) 0.0866(13) 0.0373(8) -0.0005(8) -0.0182(9) -0.0551(11) F2 0.0652(10) 0.0718(11) 0.0568(10) -0.0121(8) 0.0340(8) -0.0202(9) F3 0.0955(12) 0.0407(8) 0.0501(9) 0.0084(7) 0.0044(8) -0.0352(8) S1 0.0309(2) 0.0187(2) 0.0285(2) -0.00517(17) 0.00497(18) -0.00850(18) C18 0.0655(15) 0.0384(12) 0.0348(12) -0.0119(10) 0.0119(11) -0.0172(11) C9 0.0454(14) 0.0686(18) 0.0565(16) -0.0262(14) 0.0165(12) -0.0181(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.1434(17) . ? Ag1 N1 2.1444(18) . ? Ag1 Ag1 3.2458(8) 2_666 ? C1 N1 1.342(2) . ? C1 C5 1.388(3) . ? C1 H1 0.9500 . ? C10 N2 1.338(2) . ? C10 C14 1.386(3) . ? C10 H10 0.9500 . ? C14 C13 1.392(3) . ? C14 C15 1.490(3) . ? C11 N2 1.349(2) . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C2 N1 1.350(2) . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.492(3) . ? C15 O4 1.202(2) . ? C15 O5 1.329(2) . ? C6 O1 1.200(2) . ? C6 O2 1.340(2) . ? C19 F2 1.317(3) . ? C19 F1 1.324(3) . ? C19 F3 1.332(3) . ? C19 S1 1.824(2) . ? C7 O2 1.460(2) . ? C7 C8 1.500(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.413(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C17 O6 1.399(3) . ? C17 C16 1.492(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C16 O5 1.459(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O8 S1 1.4431(16) . ? O9 S1 1.4422(14) . ? O7 S1 1.4318(16) . ? O3 C9 1.418(3) . ? O6 C18 1.423(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 N2 Ag1 N1 171.92(6) . . ? N2 Ag1 Ag1 98.63(5) . 2_666 ? N1 Ag1 Ag1 89.19(5) . 2_666 ? N1 C1 C5 122.52(17) . . ? N1 C1 H1 118.7 . . ? C5 C1 H1 118.7 . . ? N2 C10 C14 122.63(17) . . ? N2 C10 H10 118.7 . . ? C14 C10 H10 118.7 . . ? C10 C14 C13 118.89(17) . . ? C10 C14 C15 117.25(17) . . ? C13 C14 C15 123.79(17) . . ? N2 C11 C12 122.45(18) . . ? N2 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 119.30(17) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 118.56(17) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? N1 C2 C3 122.03(18) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 119.66(18) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.64(17) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C1 C5 C4 118.67(17) . . ? C1 C5 C6 117.34(17) . . ? C4 C5 C6 123.93(17) . . ? O4 C15 O5 124.35(18) . . ? O4 C15 C14 123.83(18) . . ? O5 C15 C14 111.77(16) . . ? O1 C6 O2 124.74(18) . . ? O1 C6 C5 123.34(18) . . ? O2 C6 C5 111.85(17) . . ? F2 C19 F1 108.3(2) . . ? F2 C19 F3 107.5(2) . . ? F1 C19 F3 107.7(2) . . ? F2 C19 S1 111.32(17) . . ? F1 C19 S1 111.23(17) . . ? F3 C19 S1 110.66(16) . . ? O2 C7 C8 108.24(18) . . ? O2 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O2 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O3 C8 C7 109.99(17) . . ? O3 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O6 C17 C16 108.35(18) . . ? O6 C17 H17A 110.0 . . ? C16 C17 H17A 110.0 . . ? O6 C17 H17B 110.0 . . ? C16 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? O5 C16 C17 107.60(18) . . ? O5 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? O5 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C10 N2 C11 118.14(16) . . ? C10 N2 Ag1 120.17(12) . . ? C11 N2 Ag1 121.68(13) . . ? C1 N1 C2 118.43(16) . . ? C1 N1 Ag1 119.67(12) . . ? C2 N1 Ag1 121.89(13) . . ? C15 O5 C16 114.14(16) . . ? C6 O2 C7 115.02(16) . . ? C8 O3 C9 111.36(18) . . ? C17 O6 C18 112.13(18) . . ? O7 S1 O9 114.80(10) . . ? O7 S1 O8 115.41(11) . . ? O9 S1 O8 113.70(10) . . ? O7 S1 C19 103.70(11) . . ? O9 S1 C19 103.83(10) . . ? O8 S1 C19 103.31(10) . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C10 C14 C13 1.2(3) . . . . ? N2 C10 C14 C15 -175.92(16) . . . . ? N2 C11 C12 C13 0.7(3) . . . . ? C11 C12 C13 C14 1.0(3) . . . . ? C10 C14 C13 C12 -1.9(3) . . . . ? C15 C14 C13 C12 175.04(17) . . . . ? N1 C2 C3 C4 1.6(3) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? N1 C1 C5 C4 1.9(3) . . . . ? N1 C1 C5 C6 -175.51(16) . . . . ? C3 C4 C5 C1 -2.2(3) . . . . ? C3 C4 C5 C6 175.11(17) . . . . ? C10 C14 C15 O4 -10.4(3) . . . . ? C13 C14 C15 O4 172.61(19) . . . . ? C10 C14 C15 O5 167.21(16) . . . . ? C13 C14 C15 O5 -9.8(3) . . . . ? C1 C5 C6 O1 13.5(3) . . . . ? C4 C5 C6 O1 -163.83(19) . . . . ? C1 C5 C6 O2 -169.26(16) . . . . ? C4 C5 C6 O2 13.4(3) . . . . ? O2 C7 C8 O3 84.8(2) . . . . ? O6 C17 C16 O5 -70.8(2) . . . . ? C14 C10 N2 C11 0.5(3) . . . . ? C14 C10 N2 Ag1 179.18(13) . . . . ? C12 C11 N2 C10 -1.4(3) . . . . ? C12 C11 N2 Ag1 179.85(15) . . . . ? N1 Ag1 N2 C10 -106.7(4) . . . . ? Ag1 Ag1 N2 C10 58.58(14) 2_666 . . . ? N1 Ag1 N2 C11 72.0(5) . . . . ? Ag1 Ag1 N2 C11 -122.74(14) 2_666 . . . ? C5 C1 N1 C2 0.1(3) . . . . ? C5 C1 N1 Ag1 179.00(13) . . . . ? C3 C2 N1 C1 -1.9(3) . . . . ? C3 C2 N1 Ag1 179.21(14) . . . . ? N2 Ag1 N1 C1 -82.6(4) . . . . ? Ag1 Ag1 N1 C1 112.00(13) 2_666 . . . ? N2 Ag1 N1 C2 96.3(4) . . . . ? Ag1 Ag1 N1 C2 -69.14(14) 2_666 . . . ? O4 C15 O5 C16 2.8(3) . . . . ? C14 C15 O5 C16 -174.82(16) . . . . ? C17 C16 O5 C15 170.10(18) . . . . ? O1 C6 O2 C7 4.9(3) . . . . ? C5 C6 O2 C7 -172.31(15) . . . . ? C8 C7 O2 C6 177.50(16) . . . . ? C7 C8 O3 C9 -175.6(2) . . . . ? C16 C17 O6 C18 179.38(18) . . . . ? F2 C19 S1 O7 178.00(16) . . . . ? F1 C19 S1 O7 -61.07(19) . . . . ? F3 C19 S1 O7 58.57(19) . . . . ? F2 C19 S1 O9 -61.69(19) . . . . ? F1 C19 S1 O9 59.24(19) . . . . ? F3 C19 S1 O9 178.87(16) . . . . ? F2 C19 S1 O8 57.23(19) . . . . ? F1 C19 S1 O8 178.16(17) . . . . ? F3 C19 S1 O8 -62.20(19) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.345 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.055 # Attachment '4361_web_deposit_cif_file_3_FabienneGschwind_1298368545.cif' data_23b _database_code_depnum_ccdc_archive 'CCDC 814123' #TrackingRef '4361_web_deposit_cif_file_3_FabienneGschwind_1298368545.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'silver triflatre monomethyl diethylene glycol' _chemical_formula_moiety 'C22 H30 Ag N2 O8, C F3 O3 S' _chemical_formula_sum 'C23 H30 Ag F3 N2 O11 S' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 707.42 # start Validation Reply Form _vrf_PLAT222_23b ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.72 Ratio RESPONSE: poor crystal quality ; # end Validation Reply Form 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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9425(14) _cell_length_b 14.521(3) _cell_length_c 15.221(3) _cell_angle_alpha 65.67(3) _cell_angle_beta 85.39(3) _cell_angle_gamma 89.13(3) _cell_volume 1393.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5674 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.43 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65311 _exptl_absorpt_correction_T_max 1.75863 _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20178 _diffrn_reflns_av_R_equivalents 0.1492 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.43 _reflns_number_total 5647 _reflns_number_gt 4611 _reflns_threshold_expression >2\s(I) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material Word _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^ > 2\s(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^)+(0.0844P)^2^+38.8316P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5647 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1489 _refine_ls_R_factor_gt 0.1309 _refine_ls_wR_factor_ref 0.3281 _refine_ls_wR_factor_gt 0.3167 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 C1 C 0.6869(17) 0.5719(9) 0.2929(8) 0.027(2) Uani 1 1 d . . . H1 H 0.7061 0.5020 0.3093 0.032 Uiso 1 1 calc R . . C2 C 0.6798(18) 0.7071(10) 0.3348(10) 0.037(3) Uani 1 1 d . . . H2 H 0.6971 0.7337 0.3812 0.044 Uiso 1 1 calc R . . C3 C 0.6371(19) 0.7737(11) 0.2424(11) 0.040(3) Uani 1 1 d . . . H3 H 0.6193 0.8436 0.2266 0.048 Uiso 1 1 calc R . . C4 C 0.6219(17) 0.7348(9) 0.1754(9) 0.032(3) Uani 1 1 d . . . H4 H 0.5924 0.7778 0.1116 0.039 Uiso 1 1 calc R . . C5 C 0.6494(17) 0.6325(9) 0.2002(10) 0.032(3) Uani 1 1 d . . . C6 C 0.6296(16) 0.5912(9) 0.1268(9) 0.031(3) Uani 1 1 d . . . C7 C 0.6744(19) 0.4498(10) 0.0874(10) 0.035(3) Uani 1 1 d . . . H7A H 0.7337 0.4922 0.0219 0.043 Uiso 1 1 calc R . . H7B H 0.5353 0.4403 0.0828 0.043 Uiso 1 1 calc R . . C8 C 0.7692(17) 0.3502(10) 0.1259(10) 0.034(3) Uani 1 1 d . . . H8A H 0.7450 0.3173 0.1972 0.041 Uiso 1 1 calc R . . H8B H 0.7158 0.3057 0.0987 0.041 Uiso 1 1 calc R . . C9 C 1.073(2) 0.2727(11) 0.1239(10) 0.038(3) Uani 1 1 d . . . H9A H 1.1928 0.2843 0.0809 0.045 Uiso 1 1 calc R . . H9B H 0.9897 0.2245 0.1124 0.045 Uiso 1 1 calc R . . C10 C 1.1231(19) 0.2258(11) 0.2283(10) 0.039(3) Uani 1 1 d . . . H10A H 1.0109 0.2289 0.2714 0.046 Uiso 1 1 calc R . . H10B H 1.1562 0.1540 0.2470 0.046 Uiso 1 1 calc R . . C11 C 1.344(3) 0.2387(16) 0.3332(14) 0.066(5) Uani 1 1 d . . . H11A H 1.4537 0.2789 0.3358 0.098 Uiso 1 1 calc R . . H11B H 1.3835 0.1687 0.3506 0.098 Uiso 1 1 calc R . . H11C H 1.2375 0.2403 0.3789 0.098 Uiso 1 1 calc R . . C12 C 0.8274(17) 0.3513(9) 0.7139(10) 0.032(3) Uani 1 1 d . . . H12 H 0.8192 0.3044 0.6855 0.039 Uiso 1 1 calc R . . C13 C 0.8176(18) 0.5147(10) 0.7019(10) 0.033(3) Uani 1 1 d . . . H13 H 0.7998 0.5846 0.6641 0.040 Uiso 1 1 calc R . . C14 C 0.8529(18) 0.4850(12) 0.7968(10) 0.040(3) Uani 1 1 d . . . H14 H 0.8612 0.5334 0.8235 0.048 Uiso 1 1 calc R . . C15 C 0.8761(18) 0.3850(12) 0.8523(10) 0.041(3) Uani 1 1 d . . . H15 H 0.9026 0.3626 0.9181 0.049 Uiso 1 1 calc R . . C16 C 0.8604(15) 0.3166(9) 0.8114(9) 0.029(3) Uani 1 1 d . . . C17 C 0.8854(17) 0.2078(10) 0.8732(10) 0.035(3) Uani 1 1 d . . . C18 C 0.872(3) 0.0409(13) 0.884(2) 0.091(8) Uani 1 1 d . . . H18A H 0.9986 0.0252 0.8592 0.109 Uiso 1 1 calc R . . H18B H 0.8820 0.0272 0.9532 0.109 Uiso 1 1 calc R . . C19 C 0.736(3) -0.0220(15) 0.880(2) 0.108(10) Uani 1 1 d . . . H19A H 0.7798 -0.0314 0.8203 0.129 Uiso 1 1 calc R . . H19B H 0.7601 -0.0872 0.9339 0.129 Uiso 1 1 calc R . . C20 C 0.449(3) -0.0941(13) 0.8703(14) 0.060(4) Uani 1 1 d . . . H20A H 0.3372 -0.1133 0.9191 0.073 Uiso 1 1 calc R . . H20B H 0.5322 -0.1540 0.8862 0.073 Uiso 1 1 calc R . . C21 C 0.378(2) -0.0699(13) 0.7750(15) 0.060(4) Uani 1 1 d . . . H21A H 0.4887 -0.0542 0.7257 0.072 Uiso 1 1 calc R . . H21B H 0.3074 -0.1295 0.7767 0.072 Uiso 1 1 calc R . . C22 C 0.189(4) 0.0398(19) 0.655(2) 0.122(12) Uani 1 1 d . . . H22A H 0.1040 0.0979 0.6412 0.183 Uiso 1 1 calc R . . H22B H 0.1165 -0.0168 0.6531 0.183 Uiso 1 1 calc R . . H22C H 0.2990 0.0584 0.6060 0.183 Uiso 1 1 calc R . . C23 C 0.746(2) 0.1628(13) 0.5269(12) 0.054(4) Uani 1 1 d . . . N1 N 0.6980(15) 0.6054(9) 0.3620(9) 0.038(2) Uani 1 1 d . . . N2 N 0.8068(15) 0.4506(8) 0.6595(8) 0.037(2) Uani 1 1 d . . . O1 O 0.5568(13) 0.6374(7) 0.0492(7) 0.039(2) Uani 1 1 d . . . O2 O 0.6977(13) 0.4998(7) 0.1521(6) 0.035(2) Uani 1 1 d . . . O3 O 0.9748(12) 0.3659(7) 0.0992(7) 0.038(2) Uani 1 1 d . . . O4 O 1.2819(14) 0.2796(8) 0.2376(8) 0.049(3) Uani 1 1 d . . . O5 O 0.9465(17) 0.1778(9) 0.9533(8) 0.060(3) Uani 1 1 d . . . O6 O 0.8371(17) 0.1475(7) 0.8316(9) 0.059(3) Uani 1 1 d . . . O7 O 0.551(3) -0.0200(11) 0.8791(17) 0.121(8) Uani 1 1 d . . . O8 O 0.258(2) 0.0103(11) 0.7496(15) 0.104(6) Uani 1 1 d . . . O9 O 0.620(2) 0.3451(6) 0.4971(7) 0.057(3) Uani 1 1 d . . . O10 O 0.9911(16) 0.3038(8) 0.5107(7) 0.053(3) Uani 1 1 d . . . O11 O 0.8307(15) 0.3176(8) 0.3695(7) 0.045(2) Uani 1 1 d . . . F1 F 0.579(2) 0.1427(10) 0.5042(10) 0.102(5) Uani 1 1 d . . . F2 F 0.884(2) 0.1079(8) 0.5063(10) 0.089(4) Uani 1 1 d . . . F3 F 0.7264(18) 0.1312(9) 0.6235(7) 0.080(3) Uani 1 1 d . . . S1 S 0.8098(5) 0.2964(3) 0.4708(3) 0.0390(8) Uani 1 1 d . . . Ag1 Ag 0.75566(15) 0.51207(8) 0.50763(7) 0.0353(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 C1 0.031(6) 0.025(6) 0.024(6) -0.009(5) -0.001(4) 0.001(5) C2 0.031(6) 0.032(6) 0.047(8) -0.016(6) -0.003(6) -0.002(5) C3 0.032(6) 0.037(7) 0.055(9) -0.023(7) -0.006(6) 0.004(5) C4 0.030(6) 0.026(6) 0.030(6) -0.001(5) -0.003(5) 0.002(5) C5 0.024(6) 0.031(6) 0.041(7) -0.014(6) -0.011(5) 0.006(5) C6 0.019(5) 0.034(6) 0.038(7) -0.015(5) 0.000(5) 0.004(5) C7 0.036(7) 0.041(7) 0.038(7) -0.024(6) -0.012(5) 0.004(5) C8 0.029(6) 0.036(7) 0.038(7) -0.016(6) -0.007(5) -0.003(5) C9 0.037(7) 0.042(7) 0.034(7) -0.015(6) -0.006(5) 0.004(6) C10 0.030(6) 0.041(7) 0.036(7) -0.007(6) -0.001(5) 0.001(5) C11 0.059(10) 0.081(13) 0.073(12) -0.045(11) -0.026(9) 0.023(9) C12 0.026(6) 0.026(6) 0.045(7) -0.013(5) -0.009(5) -0.002(5) C13 0.030(6) 0.032(6) 0.039(7) -0.016(6) 0.003(5) -0.009(5) C14 0.029(6) 0.057(9) 0.045(8) -0.032(7) 0.007(6) -0.009(6) C15 0.025(6) 0.065(9) 0.033(7) -0.019(7) -0.012(5) -0.010(6) C16 0.016(5) 0.030(6) 0.033(6) -0.003(5) -0.007(4) -0.005(4) C17 0.024(6) 0.034(7) 0.036(7) -0.003(5) -0.005(5) -0.004(5) C18 0.105(17) 0.034(9) 0.15(2) -0.037(12) -0.083(16) 0.034(10) C19 0.054(12) 0.043(11) 0.17(3) 0.008(13) -0.017(14) 0.006(9) C20 0.067(11) 0.045(9) 0.064(11) -0.016(8) -0.006(9) 0.001(8) C21 0.047(9) 0.050(9) 0.087(13) -0.031(9) -0.012(9) -0.002(7) C22 0.12(2) 0.072(15) 0.14(3) 0.005(16) -0.065(19) -0.036(15) C23 0.055(9) 0.052(9) 0.048(9) -0.010(7) -0.012(7) -0.019(8) N1 0.029(5) 0.041(6) 0.046(7) -0.022(5) -0.001(5) -0.002(5) N2 0.024(5) 0.035(6) 0.045(6) -0.011(5) -0.002(5) -0.003(4) O1 0.035(5) 0.047(5) 0.031(5) -0.010(4) -0.010(4) 0.002(4) O2 0.038(5) 0.040(5) 0.033(5) -0.018(4) -0.011(4) 0.001(4) O3 0.029(4) 0.039(5) 0.044(5) -0.014(4) -0.006(4) -0.004(4) O4 0.035(5) 0.061(7) 0.046(6) -0.016(5) -0.008(4) -0.005(5) O5 0.062(7) 0.063(7) 0.043(6) -0.006(5) -0.025(5) 0.003(6) O6 0.065(7) 0.031(5) 0.080(8) -0.015(5) -0.054(6) 0.011(5) O7 0.120(14) 0.054(9) 0.20(2) -0.054(11) -0.105(15) 0.023(9) O8 0.095(11) 0.068(9) 0.165(17) -0.052(10) -0.088(12) 0.028(8) O9 0.121(10) 0.015(4) 0.033(5) -0.011(4) 0.022(6) -0.006(5) O10 0.058(6) 0.054(6) 0.038(6) -0.008(5) -0.003(5) -0.027(5) O11 0.055(6) 0.046(6) 0.027(5) -0.009(4) -0.004(4) -0.004(5) F1 0.105(9) 0.082(8) 0.095(9) -0.005(7) -0.039(8) -0.060(7) F2 0.118(10) 0.049(6) 0.103(10) -0.035(6) -0.012(8) 0.017(6) F3 0.096(8) 0.074(7) 0.042(6) 0.006(5) -0.010(5) -0.018(6) S1 0.0408(18) 0.0386(18) 0.0386(18) -0.0175(15) 0.0003(14) -0.0081(14) Ag1 0.0361(5) 0.0389(6) 0.0276(5) -0.0102(4) -0.0050(4) 0.0004(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.336(16) . ? C1 C5 1.366(17) . ? C1 H1 0.9500 . ? C2 N1 1.366(17) . ? C2 C3 1.39(2) . ? C2 H2 0.9500 . ? C3 C4 1.366(19) . ? C3 H3 0.9500 . ? C4 C5 1.388(17) . ? C4 H4 0.9500 . ? C5 C6 1.484(18) . ? C6 O1 1.238(15) . ? C6 O2 1.313(15) . ? C7 O2 1.462(15) . ? C7 C8 1.484(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.447(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O3 1.423(16) . ? C9 C10 1.517(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O4 1.411(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O4 1.43(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.347(16) . ? C12 C16 1.394(18) . ? C12 H12 0.9500 . ? C13 N2 1.341(17) . ? C13 C14 1.369(19) . ? C13 H13 0.9500 . ? C14 C15 1.36(2) . ? C14 H14 0.9500 . ? C15 C16 1.382(19) . ? C15 H15 0.9500 . ? C16 C17 1.485(17) . ? C17 O5 1.223(16) . ? C17 O6 1.335(17) . ? C18 C19 1.35(3) . ? C18 O6 1.448(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O7 1.29(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O7 1.35(2) . ? C20 C21 1.47(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O8 1.36(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O8 1.44(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 F1 1.307(18) . ? C23 F3 1.344(19) . ? C23 F2 1.34(2) . ? C23 S1 1.813(17) . ? N1 Ag1 2.136(12) . ? N2 Ag1 2.165(12) . ? O9 S1 1.583(12) . ? O10 S1 1.465(11) . ? O11 S1 1.438(10) . ? 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 C1 C5 123.6(11) . . ? N1 C1 H1 118.2 . . ? C5 C1 H1 118.2 . . ? N1 C2 C3 123.3(13) . . ? N1 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? C4 C3 C2 117.5(12) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 120.1(12) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C1 C5 C4 118.7(12) . . ? C1 C5 C6 121.8(11) . . ? C4 C5 C6 119.4(11) . . ? O1 C6 O2 122.6(12) . . ? O1 C6 C5 124.2(11) . . ? O2 C6 C5 113.3(10) . . ? O2 C7 C8 109.2(10) . . ? O2 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O2 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O3 C8 C7 108.6(11) . . ? O3 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? O3 C9 C10 113.2(11) . . ? O3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? O3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.8 . . ? O4 C10 C9 108.8(11) . . ? O4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C16 120.8(12) . . ? N2 C12 H12 119.6 . . ? C16 C12 H12 119.6 . . ? N2 C13 C14 123.5(13) . . ? N2 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C15 C14 C13 118.9(13) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 118.9(12) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C12 119.6(11) . . ? C15 C16 C17 118.2(12) . . ? C12 C16 C17 122.2(12) . . ? O5 C17 O6 124.2(13) . . ? O5 C17 C16 122.8(13) . . ? O6 C17 C16 113.0(11) . . ? C19 C18 O6 114.9(15) . . ? C19 C18 H18A 108.5 . . ? O6 C18 H18A 108.5 . . ? C19 C18 H18B 108.5 . . ? O6 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O7 C19 C18 134(2) . . ? O7 C19 H19A 103.6 . . ? C18 C19 H19A 103.6 . . ? O7 C19 H19B 103.6 . . ? C18 C19 H19B 103.6 . . ? H19A C19 H19B 105.3 . . ? O7 C20 C21 116.3(16) . . ? O7 C20 H20A 108.2 . . ? C21 C20 H20A 108.2 . . ? O7 C20 H20B 108.2 . . ? C21 C20 H20B 108.2 . . ? H20A C20 H20B 107.4 . . ? O8 C21 C20 111.5(17) . . ? O8 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? O8 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? F1 C23 F3 105.0(14) . . ? F1 C23 F2 110.1(16) . . ? F3 C23 F2 107.4(15) . . ? F1 C23 S1 113.1(13) . . ? F3 C23 S1 109.6(12) . . ? F2 C23 S1 111.3(12) . . ? C1 N1 C2 116.6(12) . . ? C1 N1 Ag1 124.3(9) . . ? C2 N1 Ag1 119.0(9) . . ? C12 N2 C13 118.1(12) . . ? C12 N2 Ag1 123.7(9) . . ? C13 N2 Ag1 118.3(9) . . ? C6 O2 C7 117.6(10) . . ? C9 O3 C8 111.8(10) . . ? C10 O4 C11 112.8(13) . . ? C17 O6 C18 116.1(12) . . ? C19 O7 C20 122(2) . . ? C21 O8 C22 114(2) . . ? O11 S1 O10 114.0(6) . . ? O11 S1 O9 111.2(6) . . ? O10 S1 O9 119.8(7) . . ? O11 S1 C23 102.8(7) . . ? O10 S1 C23 104.6(7) . . ? O9 S1 C23 101.8(7) . . ? N1 Ag1 N2 166.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -3(2) . . . . ? C2 C3 C4 C5 -0.3(19) . . . . ? N1 C1 C5 C4 0.3(19) . . . . ? N1 C1 C5 C6 -177.2(11) . . . . ? C3 C4 C5 C1 1.6(18) . . . . ? C3 C4 C5 C6 179.2(11) . . . . ? C1 C5 C6 O1 164.1(12) . . . . ? C4 C5 C6 O1 -13.4(18) . . . . ? C1 C5 C6 O2 -15.9(16) . . . . ? C4 C5 C6 O2 166.6(11) . . . . ? O2 C7 C8 O3 -80.5(13) . . . . ? O3 C9 C10 O4 -75.4(14) . . . . ? N2 C13 C14 C15 -0.9(19) . . . . ? C13 C14 C15 C16 -0.9(19) . . . . ? C14 C15 C16 C12 2.0(18) . . . . ? C14 C15 C16 C17 -179.8(11) . . . . ? N2 C12 C16 C15 -1.3(18) . . . . ? N2 C12 C16 C17 -179.5(11) . . . . ? C15 C16 C17 O5 -11.0(19) . . . . ? C12 C16 C17 O5 167.2(13) . . . . ? C15 C16 C17 O6 169.9(12) . . . . ? C12 C16 C17 O6 -11.9(17) . . . . ? O6 C18 C19 O7 -38(5) . . . . ? O7 C20 C21 O8 -60(2) . . . . ? C5 C1 N1 C2 -3.3(18) . . . . ? C5 C1 N1 Ag1 179.8(9) . . . . ? C3 C2 N1 C1 4.8(18) . . . . ? C3 C2 N1 Ag1 -178.2(10) . . . . ? C16 C12 N2 C13 -0.5(17) . . . . ? C16 C12 N2 Ag1 179.9(8) . . . . ? C14 C13 N2 C12 1.6(18) . . . . ? C14 C13 N2 Ag1 -178.7(10) . . . . ? O1 C6 O2 C7 -3.7(17) . . . . ? C5 C6 O2 C7 176.3(10) . . . . ? C8 C7 O2 C6 177.0(11) . . . . ? C10 C9 O3 C8 -83.9(13) . . . . ? C7 C8 O3 C9 -173.2(10) . . . . ? C9 C10 O4 C11 -178.1(12) . . . . ? O5 C17 O6 C18 -4(2) . . . . ? C16 C17 O6 C18 175.3(16) . . . . ? C19 C18 O6 C17 142(2) . . . . ? C18 C19 O7 C20 178(3) . . . . ? C21 C20 O7 C19 -104(3) . . . . ? C20 C21 O8 C22 177.8(18) . . . . ? F1 C23 S1 O11 -64.9(16) . . . . ? F3 C23 S1 O11 178.4(12) . . . . ? F2 C23 S1 O11 59.7(13) . . . . ? F1 C23 S1 O10 175.8(14) . . . . ? F3 C23 S1 O10 59.0(14) . . . . ? F2 C23 S1 O10 -59.6(13) . . . . ? F1 C23 S1 O9 50.4(16) . . . . ? F3 C23 S1 O9 -66.3(13) . . . . ? F2 C23 S1 O9 175.0(11) . . . . ? C1 N1 Ag1 N2 -178.9(14) . . . . ? C2 N1 Ag1 N2 4(2) . . . . ? C12 N2 Ag1 N1 174.2(14) . . . . ? C13 N2 Ag1 N1 -5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.474 _refine_diff_density_min -1.866 _refine_diff_density_rms 0.249