# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _publ_section_title ;Molecular tectonics: generation of 1-D interdigitated and 2-D interwoven helical silver coordination networks by oligoethylene glycol based tectons bearing two benzonitrile moieties ; _publ_contact_author_name 'Prof. M.Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR loop_ _publ_author_name M.Hosseini 'Julien Bourlier' 'Nathalie Kyritsakas' 'Jean-Marc Planeix' # Attachment 'New CIF For 1-AgSbF6.cif' data_e299a _database_code_depnum_ccdc_archive 'CCDC 624584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Ag N3 O3, F6 Sb' _chemical_formula_sum 'C24 H18 Ag F6 N3 O3 Sb' _chemical_formula_weight 740.03 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0108(2) _cell_length_b 11.0338(3) _cell_length_c 16.9120(4) _cell_angle_alpha 93.6370(10) _cell_angle_beta 95.7360(10) _cell_angle_gamma 95.7290(10) _cell_volume 1291.62(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7459 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 29.97 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8956 _exptl_absorpt_correction_T_max 0.9286 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 33992 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7529 _reflns_number_gt 6528 _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^)+(0.0289P)^2^+0.5120P] 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 7529 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.78730(2) -0.050001(14) 0.056301(8) 0.03539(4) Uani 1 1 d . . . C1 C 0.9229(2) 0.27170(15) 0.25913(9) 0.0225(3) Uani 1 1 d . . . C2 C 0.9050(3) 0.27012(16) 0.34117(10) 0.0253(3) Uani 1 1 d . . . H2 H 0.8625 0.1964 0.3633 0.030 Uiso 1 1 calc R . . C3 C 0.9504(2) 0.37729(16) 0.38907(9) 0.0248(3) Uani 1 1 d . . . H3 H 0.9394 0.3772 0.4446 0.030 Uiso 1 1 calc R . . C4 C 1.0122(2) 0.48603(15) 0.35655(9) 0.0213(3) Uani 1 1 d . . . C5 C 1.0332(2) 0.48742(15) 0.27541(9) 0.0235(3) Uani 1 1 d . . . H5 H 1.0776 0.5609 0.2535 0.028 Uiso 1 1 calc R . . C6 C 0.9882(2) 0.37980(16) 0.22724(9) 0.0235(3) Uani 1 1 d . . . H6 H 1.0020 0.3797 0.1719 0.028 Uiso 1 1 calc R . . C7 C 0.8725(3) 0.16388(16) 0.20597(10) 0.0270(3) Uani 1 1 d . . . N1 N 0.8320(3) 0.08129(15) 0.16103(10) 0.0351(4) Uani 1 1 d . . . O1 O 1.0498(2) 0.58527(11) 0.41039(7) 0.0289(3) Uani 1 1 d . . . C8 C 1.1150(3) 0.70384(16) 0.38688(11) 0.0308(4) Uani 1 1 d . . . H8A H 1.2012 0.6943 0.3445 0.037 Uiso 1 1 calc R . . H8B H 1.1910 0.7516 0.4331 0.037 Uiso 1 1 calc R . . C9 C 0.9517(3) 0.77405(18) 0.35673(11) 0.0348(4) Uani 1 1 d . . . H9A H 0.8374 0.7531 0.3851 0.042 Uiso 1 1 calc R . . H9B H 0.9905 0.8629 0.3665 0.042 Uiso 1 1 calc R . . O2 O 0.9057(2) 0.74237(12) 0.27261(7) 0.0310(3) Uani 1 1 d . . . C10 C 0.7374(3) 0.77128(15) 0.23579(10) 0.0243(3) Uani 1 1 d . . . C11 C 0.6960(3) 0.72543(15) 0.15585(10) 0.0247(3) Uani 1 1 d . . . H11 H 0.7849 0.6797 0.1314 0.030 Uiso 1 1 calc R . . C12 C 0.5257(3) 0.74685(15) 0.11263(10) 0.0257(3) Uani 1 1 d . . . H12 H 0.4965 0.7149 0.0588 0.031 Uiso 1 1 calc R . . C13 C 0.3964(3) 0.81618(16) 0.14906(11) 0.0268(3) Uani 1 1 d . . . C14 C 0.4377(3) 0.86069(16) 0.22855(11) 0.0304(4) Uani 1 1 d . . . H14 H 0.3488 0.9065 0.2530 0.037 Uiso 1 1 calc R . . C15 C 0.6075(3) 0.83875(16) 0.27242(11) 0.0295(4) Uani 1 1 d . . . H15 H 0.6351 0.8692 0.3266 0.035 Uiso 1 1 calc R . . C16 C 0.2238(3) 0.84510(17) 0.10417(12) 0.0320(4) Uani 1 1 d . . . N2 N 0.0894(3) 0.87398(16) 0.06902(12) 0.0411(4) Uani 1 1 d . . . C17 C 0.5743(2) -0.26455(15) -0.18739(9) 0.0227(3) Uani 1 1 d . . . C18 C 0.5170(3) -0.38954(16) -0.18615(10) 0.0248(3) Uani 1 1 d . . . H18 H 0.4953 -0.4240 -0.1373 0.030 Uiso 1 1 calc R . . C19 C 0.4925(2) -0.46221(15) -0.25672(10) 0.0245(3) Uani 1 1 d . . . H19 H 0.4538 -0.5472 -0.2565 0.029 Uiso 1 1 calc R . . C20 C 0.5242(2) -0.41132(14) -0.32863(9) 0.0204(3) Uani 1 1 d . . . C21 C 0.5807(2) -0.28678(15) -0.33029(9) 0.0227(3) Uani 1 1 d . . . H21 H 0.6018 -0.2524 -0.3792 0.027 Uiso 1 1 calc R . . C22 C 0.6057(3) -0.21377(15) -0.25927(10) 0.0243(3) Uani 1 1 d . . . H22 H 0.6444 -0.1288 -0.2595 0.029 Uiso 1 1 calc R . . C23 C 0.6034(3) -0.18782(16) -0.11419(10) 0.0257(3) Uani 1 1 d . . . N3 N 0.6271(2) -0.12688(14) -0.05615(9) 0.0310(3) Uani 1 1 d . . . O3 O 0.49741(19) -0.49215(11) -0.39410(7) 0.0258(2) Uani 1 1 d . . . C24 C 0.5223(3) -0.44534(15) -0.46990(9) 0.0245(3) Uani 1 1 d . . . H24A H 0.6562 -0.4078 -0.4710 0.029 Uiso 1 1 calc R . . H24B H 0.4330 -0.3831 -0.4814 0.029 Uiso 1 1 calc R . . Sb1 Sb 0.0000 0.5000 0.0000 0.02183(4) Uani 1 2 d S . . F1 F 0.2049(2) 0.59054(15) -0.03992(8) 0.0547(4) Uani 1 1 d . . . F2 F -0.1587(2) 0.62217(13) -0.02386(8) 0.0546(4) Uani 1 1 d . . . F3 F 0.07688(18) 0.57753(10) 0.10202(6) 0.0336(2) Uani 1 1 d . . . Sb2 Sb 0.5000 0.0000 0.5000 0.02750(5) Uani 1 2 d S . . F4 F 0.7165(2) 0.06391(14) 0.45422(9) 0.0563(4) Uani 1 1 d . . . F5 F 0.4349(2) 0.15844(11) 0.52169(8) 0.0502(3) Uani 1 1 d . . . F6 F 0.6454(2) 0.00954(12) 0.60019(7) 0.0470(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 0.03800(8) 0.04000(8) 0.02453(7) -0.01275(6) -0.00579(5) 0.00508(6) C1 0.0224(8) 0.0252(8) 0.0191(7) -0.0036(6) 0.0006(6) 0.0027(6) C2 0.0290(8) 0.0246(8) 0.0217(7) 0.0000(6) 0.0056(6) -0.0019(6) C3 0.0303(8) 0.0290(8) 0.0142(7) -0.0004(6) 0.0043(6) -0.0014(6) C4 0.0219(7) 0.0240(7) 0.0167(7) -0.0017(6) -0.0006(5) 0.0008(6) C5 0.0273(8) 0.0257(8) 0.0169(7) 0.0031(6) 0.0003(6) 0.0021(6) C6 0.0274(8) 0.0293(8) 0.0140(6) 0.0007(6) -0.0003(6) 0.0059(6) C7 0.0299(9) 0.0296(8) 0.0213(7) -0.0026(6) 0.0015(6) 0.0051(7) N1 0.0424(9) 0.0336(8) 0.0274(8) -0.0083(6) -0.0005(7) 0.0050(7) O1 0.0425(7) 0.0231(6) 0.0181(5) -0.0032(4) -0.0012(5) -0.0029(5) C8 0.0385(10) 0.0232(8) 0.0263(8) -0.0002(6) -0.0080(7) -0.0053(7) C9 0.0494(12) 0.0281(9) 0.0247(8) -0.0042(7) -0.0050(8) 0.0070(8) O2 0.0373(7) 0.0353(7) 0.0211(6) -0.0002(5) -0.0007(5) 0.0125(6) C10 0.0328(9) 0.0191(7) 0.0214(7) 0.0025(6) 0.0032(6) 0.0043(6) C11 0.0307(9) 0.0237(8) 0.0208(7) 0.0005(6) 0.0063(6) 0.0057(6) C12 0.0312(9) 0.0234(8) 0.0224(8) 0.0014(6) 0.0042(6) 0.0020(6) C13 0.0284(9) 0.0217(8) 0.0309(9) 0.0044(6) 0.0051(7) 0.0026(6) C14 0.0386(10) 0.0248(8) 0.0306(9) 0.0020(7) 0.0105(7) 0.0102(7) C15 0.0414(10) 0.0248(8) 0.0235(8) -0.0014(6) 0.0061(7) 0.0087(7) C16 0.0316(9) 0.0239(8) 0.0410(10) 0.0027(7) 0.0056(8) 0.0026(7) N2 0.0336(9) 0.0340(9) 0.0552(11) 0.0026(8) -0.0004(8) 0.0067(7) C17 0.0234(8) 0.0263(8) 0.0174(7) -0.0046(6) -0.0002(6) 0.0031(6) C18 0.0295(8) 0.0276(8) 0.0169(7) 0.0002(6) 0.0048(6) -0.0010(6) C19 0.0295(8) 0.0222(7) 0.0208(7) -0.0005(6) 0.0042(6) -0.0018(6) C20 0.0222(7) 0.0223(7) 0.0156(6) -0.0028(5) 0.0000(5) 0.0025(6) C21 0.0294(8) 0.0221(7) 0.0161(7) 0.0000(6) 0.0005(6) 0.0037(6) C22 0.0296(8) 0.0209(7) 0.0209(7) -0.0029(6) -0.0001(6) 0.0016(6) C23 0.0276(8) 0.0276(8) 0.0208(7) -0.0013(6) -0.0001(6) 0.0022(6) N3 0.0423(9) 0.0286(7) 0.0206(7) -0.0039(6) -0.0002(6) 0.0029(6) O3 0.0388(7) 0.0220(6) 0.0152(5) -0.0034(4) 0.0021(5) 0.0008(5) C24 0.0328(9) 0.0251(8) 0.0145(7) -0.0021(6) -0.0009(6) 0.0036(6) Sb1 0.03000(8) 0.02287(7) 0.01323(7) 0.00162(5) 0.00308(5) 0.00491(6) F1 0.0522(8) 0.0779(10) 0.0287(6) 0.0055(6) 0.0090(6) -0.0246(7) F2 0.0752(10) 0.0460(7) 0.0430(7) -0.0055(6) -0.0160(7) 0.0362(7) F3 0.0506(7) 0.0328(6) 0.0159(4) -0.0027(4) 0.0003(4) 0.0030(5) Sb2 0.04370(10) 0.01960(7) 0.01800(7) -0.00033(5) 0.00786(6) -0.00593(6) F4 0.0580(9) 0.0600(9) 0.0510(8) 0.0113(7) 0.0232(7) -0.0155(7) F5 0.0855(10) 0.0276(6) 0.0381(7) -0.0028(5) 0.0080(7) 0.0103(6) F6 0.0661(9) 0.0464(7) 0.0252(6) -0.0026(5) -0.0039(5) 0.0016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.1854(15) . ? Ag1 N1 2.1924(16) . ? Ag1 N2 2.3499(18) 1_645 ? C1 C6 1.395(2) . ? C1 C2 1.407(2) . ? C1 C7 1.437(2) . ? C2 C3 1.381(2) . ? C2 H2 0.9500 . ? C3 C4 1.399(2) . ? C3 H3 0.9500 . ? C4 O1 1.3658(19) . ? C4 C5 1.396(2) . ? C5 C6 1.387(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.143(2) . ? O1 C8 1.436(2) . ? C8 C9 1.510(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.440(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O2 C10 1.354(2) . ? C10 C15 1.399(2) . ? C10 C11 1.405(2) . ? C11 C12 1.386(2) . ? C11 H11 0.9500 . ? C12 C13 1.406(2) . ? C12 H12 0.9500 . ? C13 C14 1.394(3) . ? C13 C16 1.438(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.147(3) . ? N2 Ag1 2.3499(18) 1_465 ? C17 C22 1.398(2) . ? C17 C18 1.399(2) . ? C17 C23 1.440(2) . ? C18 C19 1.381(2) . ? C18 H18 0.9500 . ? C19 C20 1.400(2) . ? C19 H19 0.9500 . ? C20 O3 1.3625(18) . ? C20 C21 1.395(2) . ? C21 C22 1.389(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 N3 1.142(2) . ? O3 C24 1.4321(19) . ? C24 C24 1.515(3) 2_644 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? Sb1 F2 1.8701(12) 2_565 ? Sb1 F2 1.8701(12) . ? Sb1 F1 1.8738(12) . ? Sb1 F1 1.8738(12) 2_565 ? Sb1 F3 1.8799(10) 2_565 ? Sb1 F3 1.8800(10) . ? Sb2 F4 1.8682(13) . ? Sb2 F4 1.8682(13) 2_656 ? Sb2 F5 1.8735(12) . ? Sb2 F5 1.8735(12) 2_656 ? Sb2 F6 1.8795(12) . ? Sb2 F6 1.8795(12) 2_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 N3 Ag1 N1 152.03(6) . . ? N3 Ag1 N2 108.79(7) . 1_645 ? N1 Ag1 N2 98.46(7) . 1_645 ? C6 C1 C2 120.19(15) . . ? C6 C1 C7 118.29(15) . . ? C2 C1 C7 121.51(16) . . ? C3 C2 C1 119.00(15) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.61(14) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O1 C4 C5 125.00(15) . . ? O1 C4 C3 114.50(14) . . ? C5 C4 C3 120.50(15) . . ? C6 C5 C4 118.97(15) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C1 120.71(14) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? N1 C7 C1 177.1(2) . . ? C7 N1 Ag1 166.80(16) . . ? C4 O1 C8 121.60(13) . . ? O1 C8 C9 112.99(16) . . ? O1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? O1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? O2 C9 C8 108.46(15) . . ? O2 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? O2 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C10 O2 C9 119.21(14) . . ? O2 C10 C15 124.60(16) . . ? O2 C10 C11 114.95(15) . . ? C15 C10 C11 120.43(17) . . ? C12 C11 C10 120.09(16) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.49(16) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.14(17) . . ? C14 C13 C16 119.37(17) . . ? C12 C13 C16 120.46(17) . . ? C15 C14 C13 120.66(17) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 119.17(16) . . ? C14 C15 H15 120.4 . . ? C10 C15 H15 120.4 . . ? N2 C16 C13 176.7(2) . . ? C16 N2 Ag1 154.25(18) . 1_465 ? C22 C17 C18 120.39(14) . . ? C22 C17 C23 119.68(15) . . ? C18 C17 C23 119.92(15) . . ? C19 C18 C17 119.22(15) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.35(15) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? O3 C20 C21 124.26(14) . . ? O3 C20 C19 115.03(14) . . ? C21 C20 C19 120.71(14) . . ? C22 C21 C20 118.92(15) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C17 120.42(15) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? N3 C23 C17 179.8(2) . . ? C23 N3 Ag1 154.80(15) . . ? C20 O3 C24 117.80(12) . . ? O3 C24 C24 105.45(17) . 2_644 ? O3 C24 H24A 110.7 . . ? C24 C24 H24A 110.7 2_644 . ? O3 C24 H24B 110.7 . . ? C24 C24 H24B 110.7 2_644 . ? H24A C24 H24B 108.8 . . ? F2 Sb1 F2 180.0 2_565 . ? F2 Sb1 F1 90.06(8) 2_565 . ? F2 Sb1 F1 89.94(8) . . ? F2 Sb1 F1 89.94(8) 2_565 2_565 ? F2 Sb1 F1 90.06(8) . 2_565 ? F1 Sb1 F1 180.0 . 2_565 ? F2 Sb1 F3 90.53(5) 2_565 2_565 ? F2 Sb1 F3 89.47(5) . 2_565 ? F1 Sb1 F3 90.06(5) . 2_565 ? F1 Sb1 F3 89.94(6) 2_565 2_565 ? F2 Sb1 F3 89.47(5) 2_565 . ? F2 Sb1 F3 90.53(5) . . ? F1 Sb1 F3 89.94(5) . . ? F1 Sb1 F3 90.06(5) 2_565 . ? F3 Sb1 F3 180.0 2_565 . ? F4 Sb2 F4 180.0 . 2_656 ? F4 Sb2 F5 89.96(7) . . ? F4 Sb2 F5 90.04(7) 2_656 . ? F4 Sb2 F5 90.04(7) . 2_656 ? F4 Sb2 F5 89.96(7) 2_656 2_656 ? F5 Sb2 F5 180.00(9) . 2_656 ? F4 Sb2 F6 90.44(7) . . ? F4 Sb2 F6 89.57(7) 2_656 . ? F5 Sb2 F6 89.72(6) . . ? F5 Sb2 F6 90.28(6) 2_656 . ? F4 Sb2 F6 89.56(7) . 2_656 ? F4 Sb2 F6 90.43(7) 2_656 2_656 ? F5 Sb2 F6 90.28(6) . 2_656 ? F5 Sb2 F6 89.73(6) 2_656 2_656 ? F6 Sb2 F6 180.0 . 2_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.798 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.076 # Attachment 'New CIF For 3-AgSbF6.cif' data_3-AgSbF6 _database_code_depnum_ccdc_archive 'CCDC 624585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Ag N2 O4, As F6' _chemical_formula_sum 'C20 H20 Ag As F6 N2 O4' _chemical_formula_weight 649.17 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' As As 0.0499 2.0058 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1230(6) _cell_length_b 11.6240(6) _cell_length_c 12.4770(9) _cell_angle_alpha 62.419(2) _cell_angle_beta 83.793(2) _cell_angle_gamma 83.386(5) _cell_volume 1162.71(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4637 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 2.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8715 _exptl_absorpt_correction_T_max 0.8913 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8950 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.09 _reflns_number_total 6759 _reflns_number_gt 3868 _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^)+(0.0858P)^2^+0.8103P] 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 6759 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1903 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.029 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.76972(5) 1.09620(4) 0.77916(4) 0.04048(17) Uani 1 1 d . . . N1 N 0.5545(6) 1.0917(5) 0.7110(5) 0.0481(13) Uani 1 1 d . . . C1 C 0.4816(6) 1.0923(6) 0.6436(6) 0.0386(14) Uani 1 1 d . . . C2 C 0.3935(6) 1.0999(6) 0.5516(6) 0.0353(13) Uani 1 1 d . . . C3 C 0.2902(6) 1.0097(6) 0.5769(6) 0.0371(13) Uani 1 1 d . . . H3 H 0.2729 0.9431 0.6571 0.044 Uiso 1 1 calc R . . C4 C 0.2138(6) 1.0187(5) 0.4840(5) 0.0341(13) Uani 1 1 d . . . H4 H 0.1439 0.9571 0.5003 0.041 Uiso 1 1 calc R . . C5 C 0.2370(6) 1.1158(5) 0.3674(5) 0.0314(12) Uani 1 1 d . . . C6 C 0.3420(6) 1.2057(5) 0.3441(6) 0.0377(14) Uani 1 1 d . . . H6 H 0.3593 1.2725 0.2640 0.045 Uiso 1 1 calc R . . C7 C 0.4183(6) 1.1981(6) 0.4341(6) 0.0380(14) Uani 1 1 d . . . H7 H 0.4886 1.2594 0.4175 0.046 Uiso 1 1 calc R . . O1 O 0.1550(4) 1.1169(4) 0.2811(4) 0.0386(9) Uani 1 1 d . . . C8 C 0.1672(7) 1.2280(6) 0.1629(6) 0.0465(16) Uani 1 1 d . . . H8A H 0.2717 1.2356 0.1310 0.056 Uiso 1 1 calc R . . H8B H 0.1306 1.3089 0.1682 0.056 Uiso 1 1 calc R . . C9 C 0.0757(7) 1.2080(6) 0.0807(6) 0.0467(16) Uani 1 1 d . . . O2 O 0.1875(11) 1.1247(9) 0.0468(9) 0.038(2) Uani 0.50 1 d P . . O2A O 0.1087(10) 1.0917(9) 0.0599(8) 0.0327(19) Uani 0.50 1 d P . . C10 C 0.1732(8) 1.1294(6) -0.0595(6) 0.0500(17) Uani 1 1 d . . . C11 C 0.2539(8) 1.0201(7) -0.0770(6) 0.0532(18) Uani 1 1 d . . . O3 O 0.2385(9) 0.9084(8) 0.0101(7) 0.0342(17) Uani 0.50 1 d P . . O3A O 0.3487(9) 0.9288(7) 0.0216(7) 0.0336(17) Uani 0.50 1 d P . . C12 C 0.3797(9) 0.8108(7) 0.0101(6) 0.0597(15) Uani 1 1 d . . . C13 C 0.3035(9) 0.6891(6) 0.0959(6) 0.0597(15) Uani 1 1 d . . . H13A H 0.1976 0.7005 0.0797 0.072 Uiso 1 1 calc R . . H13B H 0.3494 0.6137 0.0847 0.072 Uiso 1 1 calc R . . O4 O 0.3189(5) 0.6669(4) 0.2190(4) 0.0456(11) Uani 1 1 d . . . C14 C 0.2531(7) 0.5650(6) 0.3108(6) 0.0384(14) Uani 1 1 d . . . C15 C 0.2912(7) 0.5332(6) 0.4270(6) 0.0405(14) Uani 1 1 d . . . H15 H 0.3633 0.5797 0.4370 0.049 Uiso 1 1 calc R . . C16 C 0.2253(7) 0.4344(6) 0.5287(6) 0.0385(14) Uani 1 1 d . . . H16 H 0.2510 0.4134 0.6078 0.046 Uiso 1 1 calc R . . C17 C 0.1207(6) 0.3670(6) 0.5115(6) 0.0395(14) Uani 1 1 d . . . C18 C 0.0822(6) 0.3994(6) 0.3951(6) 0.0390(14) Uani 1 1 d . . . H18 H 0.0095 0.3537 0.3847 0.047 Uiso 1 1 calc R . . C19 C 0.1485(7) 0.4967(6) 0.2956(6) 0.0434(15) Uani 1 1 d . . . H19 H 0.1230 0.5174 0.2166 0.052 Uiso 1 1 calc R . . C20 C 0.0449(6) 0.2671(6) 0.6110(6) 0.0405(15) Uani 1 1 d . . . N2 N -0.0206(6) 0.1868(5) 0.6877(5) 0.0478(14) Uani 1 1 d . . . As As 0.72228(7) 0.44258(6) 0.17626(6) 0.03897(19) Uani 1 1 d . . . F1 F 0.8376(11) 0.4400(9) 0.0585(9) 0.0777(8) Uani 0.50 1 d P . . F2 F 0.6404(11) 0.5910(10) 0.0726(9) 0.0777(8) Uani 0.50 1 d P . . F3 F 0.5975(11) 0.3616(9) 0.1580(9) 0.0777(8) Uani 0.50 1 d P . . F4 F 0.6134(11) 0.4566(9) 0.2894(9) 0.0777(8) Uani 0.50 1 d P . . F5 F 0.8079(11) 0.3080(9) 0.2784(9) 0.0777(8) Uani 0.50 1 d P . . F6 F 0.8503(11) 0.5359(9) 0.1932(9) 0.0777(8) Uani 0.50 1 d P . . F1A F 0.7108(11) 0.2936(9) 0.1719(9) 0.0777(8) Uani 0.50 1 d P . . F2A F 0.7312(11) 0.5734(9) 0.1906(9) 0.0777(8) Uani 0.50 1 d P . . F3A F 0.5348(11) 0.4407(9) 0.2103(9) 0.0777(8) Uani 0.50 1 d P . . F4A F 0.9054(10) 0.4287(9) 0.1509(9) 0.0777(8) Uani 0.50 1 d P . . F5A F 0.6980(11) 0.5234(9) 0.0254(9) 0.0777(8) Uani 0.50 1 d P . . F6A F 0.7397(11) 0.3452(10) 0.3325(9) 0.0777(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0441(3) 0.0392(3) 0.0396(3) -0.0185(2) -0.0058(2) -0.0033(2) N1 0.042(3) 0.057(3) 0.050(4) -0.029(3) -0.001(3) -0.001(3) C1 0.032(3) 0.045(3) 0.044(4) -0.026(3) -0.002(3) 0.004(3) C2 0.026(3) 0.043(3) 0.045(4) -0.028(3) -0.002(2) 0.001(2) C3 0.034(3) 0.038(3) 0.037(3) -0.016(3) -0.002(3) 0.001(2) C4 0.036(3) 0.031(3) 0.035(3) -0.014(3) 0.000(2) -0.005(2) C5 0.032(3) 0.028(3) 0.033(3) -0.014(2) 0.003(2) -0.004(2) C6 0.036(3) 0.029(3) 0.043(4) -0.013(3) 0.004(3) -0.006(2) C7 0.030(3) 0.036(3) 0.050(4) -0.021(3) -0.003(3) -0.002(2) O1 0.047(2) 0.029(2) 0.038(2) -0.0111(18) -0.0067(19) -0.0070(17) C8 0.053(4) 0.041(3) 0.037(4) -0.008(3) -0.011(3) -0.004(3) C9 0.058(4) 0.042(3) 0.044(4) -0.026(3) -0.009(3) 0.016(3) O2 0.044(6) 0.036(5) 0.036(5) -0.021(4) -0.009(5) 0.009(4) O2A 0.038(5) 0.032(5) 0.030(5) -0.016(4) -0.006(4) 0.000(4) C10 0.073(5) 0.040(3) 0.031(3) -0.013(3) 0.011(3) -0.010(3) C11 0.058(4) 0.064(5) 0.046(4) -0.033(4) -0.017(3) 0.013(4) O3 0.038(4) 0.038(4) 0.032(5) -0.021(4) 0.002(4) -0.004(3) O3A 0.039(4) 0.034(4) 0.032(4) -0.020(4) 0.002(4) -0.002(3) C12 0.086(4) 0.045(3) 0.043(3) -0.021(2) 0.007(3) 0.008(3) C13 0.086(4) 0.045(3) 0.043(3) -0.021(2) 0.007(3) 0.008(3) O4 0.057(3) 0.038(2) 0.043(3) -0.019(2) -0.004(2) 0.001(2) C14 0.039(3) 0.034(3) 0.043(4) -0.020(3) -0.003(3) 0.006(2) C15 0.038(3) 0.042(3) 0.048(4) -0.026(3) -0.008(3) -0.001(3) C16 0.044(3) 0.040(3) 0.034(3) -0.020(3) -0.006(3) 0.003(3) C17 0.036(3) 0.034(3) 0.048(4) -0.021(3) -0.002(3) 0.005(2) C18 0.035(3) 0.043(3) 0.044(4) -0.025(3) -0.009(3) 0.006(3) C19 0.047(4) 0.048(4) 0.039(4) -0.025(3) -0.012(3) 0.013(3) C20 0.029(3) 0.046(4) 0.047(4) -0.024(3) -0.001(3) 0.007(3) N2 0.042(3) 0.057(4) 0.047(4) -0.026(3) 0.001(3) -0.005(3) As 0.0365(3) 0.0403(4) 0.0390(4) -0.0166(3) -0.0016(3) -0.0065(3) F1 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F2 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F3 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F4 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F5 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F6 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F1A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F2A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F3A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F4A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F5A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) F6A 0.080(2) 0.0728(19) 0.073(2) -0.0246(16) 0.0044(16) -0.0270(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N2 2.225(5) 1_665 ? Ag N1 2.237(6) . ? Ag O2A 2.428(9) 2_676 ? Ag O2 2.500(9) 2_676 ? Ag O3A 2.501(7) 2_676 ? Ag O3 2.598(8) 2_676 ? N1 C1 1.125(8) . ? C1 C2 1.436(9) . ? C2 C7 1.393(9) . ? C2 C3 1.394(8) . ? C3 C4 1.373(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(8) . ? C4 H4 0.9500 . ? C5 O1 1.370(7) . ? C5 C6 1.409(8) . ? C6 C7 1.347(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O1 C8 1.446(7) . ? C8 C9 1.500(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2A 1.483(10) . ? C9 O2 1.488(10) . ? O2 O2A 0.819(10) . ? O2 C10 1.322(11) . ? O2 Ag 2.500(9) 2_676 ? O2A C10 1.422(11) . ? O2A Ag 2.428(9) 2_676 ? C10 C11 1.487(9) . ? C11 O3 1.261(10) . ? C11 O3A 1.482(11) . ? O3 O3A 1.098(10) . ? O3 C12 1.615(10) . ? O3 Ag 2.598(8) 2_676 ? O3A C12 1.437(10) . ? O3A Ag 2.501(7) 2_676 ? C12 C13 1.515(10) . ? C13 O4 1.454(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O4 C14 1.354(8) . ? C14 C19 1.389(9) . ? C14 C15 1.394(9) . ? C15 C16 1.390(9) . ? C15 H15 0.9500 . ? C16 C17 1.395(8) . ? C16 H16 0.9500 . ? C17 C18 1.395(9) . ? C17 C20 1.425(9) . ? C18 C19 1.372(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 N2 1.150(8) . ? N2 Ag 2.225(5) 1_445 ? As F2A 1.624(10) . ? As F3 1.654(9) . ? As F5 1.664(10) . ? As F4A 1.670(9) . ? As F5A 1.697(10) . ? As F4 1.696(10) . ? As F3A 1.718(10) . ? As F1 1.722(10) . ? As F2 1.747(10) . ? As F6A 1.757(10) . ? As F1A 1.772(10) . ? As F6 1.773(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 N2 Ag N1 133.3(2) 1_665 . ? N2 Ag O2A 94.3(3) 1_665 2_676 ? N1 Ag O2A 123.5(3) . 2_676 ? N2 Ag O2 112.6(3) 1_665 2_676 ? N1 Ag O2 104.9(3) . 2_676 ? O2A Ag O2 19.1(2) 2_676 2_676 ? N2 Ag O3A 127.5(2) 1_665 2_676 ? N1 Ag O3A 92.9(2) . 2_676 ? O2A Ag O3A 71.3(3) 2_676 2_676 ? O2 Ag O3A 65.1(3) 2_676 2_676 ? N2 Ag O3 103.6(2) 1_665 2_676 ? N1 Ag O3 117.3(2) . 2_676 ? O2A Ag O3 62.5(3) 2_676 2_676 ? O2 Ag O3 65.0(3) 2_676 2_676 ? C1 N1 Ag 155.0(5) . . ? N1 C1 C2 176.3(7) . . ? C7 C2 C3 120.6(6) . . ? C7 C2 C1 117.7(6) . . ? C3 C2 C1 121.6(6) . . ? C4 C3 C2 118.9(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.0(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? O1 C5 C4 116.6(5) . . ? O1 C5 C6 124.4(5) . . ? C4 C5 C6 119.0(6) . . ? C7 C6 C5 120.8(6) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 119.7(6) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? C5 O1 C8 115.9(4) . . ? O1 C8 C9 107.7(5) . . ? O1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O1 C8 H8B 110.1 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O2A C9 C8 120.0(6) . . ? O2 C9 C8 97.8(6) . . ? O2A O2 C10 79.4(11) . . ? O2A O2 C9 73.7(10) . . ? C10 O2 C9 115.3(7) . . ? O2A O2 Ag 75.5(10) . 2_676 ? C10 O2 Ag 116.7(6) . 2_676 ? C9 O2 Ag 111.6(6) . 2_676 ? O2 O2A C10 66.1(10) . . ? O2 O2A C9 74.3(10) . . ? C10 O2A C9 109.7(7) . . ? O2 O2A Ag 85.4(10) . 2_676 ? C10 O2A Ag 116.2(6) . 2_676 ? C9 O2A Ag 115.6(5) . 2_676 ? O2 C10 C11 114.7(7) . . ? O2A C10 C11 113.8(6) . . ? O3 C11 C10 115.3(6) . . ? O3A C11 C10 115.9(6) . . ? C11 O3 C12 110.0(7) . . ? O3A O3 Ag 72.7(6) . 2_676 ? C11 O3 Ag 113.2(5) . 2_676 ? C12 O3 Ag 104.5(5) . 2_676 ? C12 O3A C11 108.2(7) . . ? O3 O3A Ag 82.6(6) . 2_676 ? C12 O3A Ag 115.9(5) . 2_676 ? C11 O3A Ag 109.5(5) . 2_676 ? O3A C12 C13 120.7(6) . . ? C13 C12 O3 94.1(6) . . ? O4 C13 C12 107.9(6) . . ? O4 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? O4 C13 H13B 110.4 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C14 O4 C13 117.8(5) . . ? O4 C14 C19 124.2(6) . . ? O4 C14 C15 116.0(6) . . ? C19 C14 C15 119.8(6) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.3(6) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C16 C17 C18 120.6(6) . . ? C16 C17 C20 121.7(6) . . ? C18 C17 C20 117.7(6) . . ? C19 C18 C17 120.5(6) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.8 . . ? C18 C19 C14 119.8(6) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? N2 C20 C17 176.9(7) . . ? C20 N2 Ag 152.3(5) . 1_445 ? F2A As F3 139.3(5) . . ? F2A As F5 115.7(5) . . ? F3 As F5 93.2(5) . . ? F2A As F4A 91.7(5) . . ? F3 As F4A 127.6(5) . . ? F5 As F4A 65.0(5) . . ? F2A As F5A 94.7(5) . . ? F3 As F5A 76.5(5) . . ? F5 As F5A 140.8(5) . . ? F4A As F5A 91.4(5) . . ? F2A As F4 63.1(5) . . ? F3 As F4 90.8(5) . . ? F5 As F4 89.6(5) . . ? F4A As F4 132.8(5) . . ? F5A As F4 127.6(5) . . ? F2A As F3A 92.7(5) . . ? F3 As F3A 48.9(5) . . ? F5 As F3A 109.9(5) . . ? F4A As F3A 174.4(4) . . ? F5A As F3A 91.6(5) . . ? F4 As F3A 47.3(4) . . ? F2A As F1 112.5(5) . . ? F3 As F1 92.9(5) . . ? F5 As F1 92.6(5) . . ? F4 As F1 175.5(4) . . ? F3A As F1 135.0(5) . . ? F3 As F2 91.3(5) . . ? F5 As F2 175.4(5) . . ? F4A As F2 112.9(4) . . ? F4 As F2 89.2(5) . . ? F3A As F2 72.4(4) . . ? F1 As F2 88.3(5) . . ? F2A As F6A 90.8(5) . . ? F3 As F6A 98.0(5) . . ? F4A As F6A 90.5(5) . . ? F5A As F6A 174.1(4) . . ? F3A As F6A 86.0(5) . . ? F1 As F6A 128.0(5) . . ? F2 As F6A 141.6(5) . . ? F2A As F1A 175.9(5) . . ? F5 As F1A 61.2(5) . . ? F4A As F1A 89.2(5) . . ? F5A As F1A 89.3(5) . . ? F4 As F1A 113.6(4) . . ? F3A As F1A 86.2(5) . . ? F1 As F1A 70.9(4) . . ? F2 As F1A 123.2(5) . . ? F6A As F1A 85.2(5) . . ? F3 As F6 177.4(5) . . ? F5 As F6 89.3(5) . . ? F4A As F6 54.5(5) . . ? F5A As F6 102.2(5) . . ? F4 As F6 88.2(5) . . ? F3A As F6 129.2(5) . . ? F1 As F6 87.9(5) . . ? F2 As F6 86.2(5) . . ? F6A As F6 83.5(4) . . ? F1A As F6 141.7(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.885 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.151 # Attachment 'New CIF For 4-AgAsF6.cif' data_4-AgAsF6 _database_code_depnum_ccdc_archive 'CCDC 624586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 N2 O5, As F6' _chemical_formula_sum 'C22 H24 Ag As F6 N2 O5' _chemical_formula_weight 693.22 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' F F 0.0171 0.0103 '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' As As 0.0499 2.0058 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.7680(2) _cell_length_b 25.7570(6) _cell_length_c 8.5870(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.9200(9) _cell_angle_gamma 90.00 _cell_volume 2583.83(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5101 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 2.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6753 _exptl_absorpt_correction_T_max 0.7406 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 11916 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.1700 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.04 _reflns_number_total 7520 _reflns_number_gt 3136 _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^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7520 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1806 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.25827(3) -0.164900(12) 1.15658(4) 0.04232(12) Uani 1 1 d . . . C1 C 1.0286(3) 0.08005(15) 0.7953(5) 0.0297(10) Uani 1 1 d . . . C2 C 0.9877(4) 0.03715(15) 0.7065(4) 0.0340(11) Uani 1 1 d . . . H2 H 0.9329 0.0420 0.6170 0.041 Uiso 1 1 calc R . . C3 C 1.0255(4) -0.01208(15) 0.7467(5) 0.0345(11) Uani 1 1 d . . . H3 H 0.9969 -0.0411 0.6859 0.041 Uiso 1 1 calc R . . C4 C 1.1058(4) -0.01890(15) 0.8768(5) 0.0305(10) Uani 1 1 d . . . C5 C 1.1462(3) 0.02379(15) 0.9661(4) 0.0323(10) Uani 1 1 d . . . H5 H 1.2010 0.0191 1.0557 0.039 Uiso 1 1 calc R . . C6 C 1.1071(3) 0.07273(14) 0.9250(5) 0.0306(10) Uani 1 1 d . . . H6 H 1.1346 0.1017 0.9868 0.037 Uiso 1 1 calc R . . C7 C 1.1488(4) -0.06976(17) 0.9243(5) 0.0362(11) Uani 1 1 d . . . N2 N 1.1848(3) -0.10919(13) 0.9672(4) 0.0423(10) Uani 1 1 d . . . O1 O 0.9852(2) 0.12696(10) 0.7460(3) 0.0329(7) Uani 1 1 d . . . C8 C 1.0460(4) 0.17239(14) 0.8077(5) 0.0369(11) Uani 1 1 d . . . H8A H 1.1278 0.1698 0.7920 0.044 Uiso 1 1 calc R . . H8B H 1.0409 0.1755 0.9216 0.044 Uiso 1 1 calc R . . C9 C 0.9932(3) 0.21844(14) 0.7235(5) 0.0384(11) Uani 1 1 d . . . H9A H 1.0471 0.2481 0.7355 0.046 Uiso 1 1 calc R . . H9B H 0.9758 0.2106 0.6103 0.046 Uiso 1 1 calc R . . O2 O 0.8899(2) 0.23165(9) 0.7873(3) 0.0351(7) Uani 1 1 d . . . C10 C 0.8395(3) 0.27755(14) 0.7168(4) 0.0340(11) Uani 1 1 d . . . H10A H 0.8079 0.2704 0.6068 0.041 Uiso 1 1 calc R . . H10B H 0.8983 0.3050 0.7164 0.041 Uiso 1 1 calc R . . C11 C 0.7460(3) 0.29544(14) 0.8076(5) 0.0345(11) Uani 1 1 d . . . H11A H 0.7777 0.3037 0.9169 0.041 Uiso 1 1 calc R . . H11B H 0.7096 0.3271 0.7593 0.041 Uiso 1 1 calc R . . O3 O 0.6632(2) 0.25459(9) 0.8063(3) 0.0355(7) Uani 1 1 d . . . C12 C 0.5711(4) 0.26881(15) 0.8920(5) 0.0427(12) Uani 1 1 d . . . H12A H 0.5301 0.2993 0.8428 0.051 Uiso 1 1 calc R . . H12B H 0.6010 0.2779 1.0013 0.051 Uiso 1 1 calc R . . C13 C 0.4915(4) 0.22339(16) 0.8904(5) 0.0521(13) Uani 1 1 d . . . H13A H 0.4247 0.2324 0.9450 0.062 Uiso 1 1 calc R . . H13B H 0.4635 0.2136 0.7810 0.062 Uiso 1 1 calc R . . O4 O 0.5532(3) 0.18148(10) 0.9683(3) 0.0459(8) Uani 1 1 d . . . C14 C 0.4851(4) 0.14369(17) 1.0365(5) 0.0545(14) Uani 1 1 d . . . H14A H 0.4292 0.1620 1.0942 0.065 Uiso 1 1 calc R . . H14B H 0.5356 0.1230 1.1136 0.065 Uiso 1 1 calc R . . C15 C 0.4226(4) 0.10805(17) 0.9231(5) 0.0511(13) Uani 1 1 d . . . H15A H 0.3600 0.0909 0.9711 0.061 Uiso 1 1 calc R . . H15B H 0.3885 0.1276 0.8296 0.061 Uiso 1 1 calc R . . O5 O 0.5018(2) 0.06951(10) 0.8779(3) 0.0419(8) Uani 1 1 d . . . C16 C 0.4577(4) 0.03189(15) 0.7763(5) 0.0325(10) Uani 1 1 d . . . C17 C 0.5328(4) -0.00862(15) 0.7512(5) 0.0410(11) Uani 1 1 d . . . H17 H 0.6087 -0.0087 0.8034 0.049 Uiso 1 1 calc R . . C18 C 0.4956(4) -0.04828(15) 0.6504(5) 0.0381(11) Uani 1 1 d . . . H18 H 0.5461 -0.0759 0.6334 0.046 Uiso 1 1 calc R . . C19 C 0.3862(4) -0.04823(16) 0.5741(5) 0.0352(11) Uani 1 1 d . . . C20 C 0.3119(4) -0.00794(16) 0.5996(5) 0.0405(12) Uani 1 1 d . . . H20 H 0.2363 -0.0079 0.5466 0.049 Uiso 1 1 calc R . . C21 C 0.3470(4) 0.03169(15) 0.7006(5) 0.0385(11) Uani 1 1 d . . . H21 H 0.2956 0.0589 0.7185 0.046 Uiso 1 1 calc R . . C22 C 0.3488(4) -0.08865(17) 0.4655(5) 0.0416(12) Uani 1 1 d . . . N3 N 0.3190(4) -0.12035(14) 0.3757(4) 0.0544(12) Uani 1 1 d . . . As1 As 0.21223(4) 0.147994(18) 0.37182(5) 0.04278(15) Uani 1 1 d . . . F1 F 0.1905(12) 0.1200(6) 0.5483(14) 0.100(5) Uani 0.50 1 d P . . F2 F 0.2625(17) 0.0921(8) 0.264(3) 0.090(5) Uani 0.50 1 d P . . F3 F 0.3479(2) 0.14996(10) 0.4654(4) 0.0910(11) Uani 1 1 d . . . F4 F 0.2323(14) 0.1727(5) 0.1982(13) 0.098(4) Uani 0.50 1 d P . . F5 F 0.168(2) 0.1982(10) 0.469(3) 0.083(6) Uani 0.50 1 d P . . F6 F 0.0789(3) 0.14498(11) 0.2725(4) 0.1152(13) Uani 1 1 d . . . F7 F 0.2322(15) 0.0916(6) 0.302(2) 0.070(4) Uani 0.50 1 d P . . F8 F 0.1595(13) 0.1054(6) 0.4864(14) 0.090(4) Uani 0.50 1 d P . . F9 F 0.186(2) 0.2075(10) 0.448(3) 0.091(7) Uani 0.50 1 d P . . F10 F 0.2691(12) 0.1918(4) 0.2519(13) 0.080(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0574(3) 0.02583(18) 0.0436(2) -0.00009(16) 0.00562(18) 0.00148(18) C1 0.025(3) 0.029(2) 0.036(3) 0.005(2) 0.010(2) 0.000(2) C2 0.034(3) 0.033(3) 0.033(2) -0.004(2) -0.003(2) -0.003(2) C3 0.039(3) 0.025(2) 0.039(3) -0.003(2) 0.004(2) -0.005(2) C4 0.030(3) 0.026(2) 0.036(2) 0.005(2) 0.010(2) 0.005(2) C5 0.025(3) 0.038(3) 0.034(2) 0.006(2) 0.003(2) -0.001(2) C6 0.030(3) 0.022(2) 0.040(3) -0.009(2) 0.006(2) 0.001(2) C7 0.038(3) 0.034(3) 0.040(3) -0.004(2) 0.016(2) -0.005(2) N2 0.052(3) 0.029(2) 0.046(2) 0.0032(19) 0.006(2) 0.005(2) O1 0.0271(18) 0.0246(15) 0.0457(17) 0.0003(14) -0.0005(14) 0.0004(13) C8 0.035(3) 0.026(2) 0.050(3) 0.001(2) 0.008(2) -0.002(2) C9 0.036(3) 0.029(2) 0.052(3) 0.002(2) 0.012(2) -0.001(2) O2 0.036(2) 0.0221(15) 0.0486(18) 0.0039(13) 0.0122(15) 0.0061(14) C10 0.033(3) 0.026(2) 0.044(3) 0.007(2) 0.006(2) 0.000(2) C11 0.038(3) 0.023(2) 0.043(3) 0.006(2) 0.005(2) 0.001(2) O3 0.037(2) 0.0260(16) 0.0456(17) 0.0005(14) 0.0123(15) 0.0005(14) C12 0.037(3) 0.030(3) 0.064(3) 0.002(2) 0.015(3) 0.002(2) C13 0.039(3) 0.051(3) 0.069(3) 0.005(3) 0.018(3) 0.002(3) O4 0.050(2) 0.0310(17) 0.060(2) 0.0028(16) 0.0200(17) -0.0093(16) C14 0.066(4) 0.049(3) 0.052(3) -0.005(3) 0.021(3) -0.018(3) C15 0.049(4) 0.055(3) 0.053(3) -0.025(3) 0.018(3) -0.015(3) O5 0.038(2) 0.0407(18) 0.0477(18) -0.0104(15) 0.0079(15) -0.0080(16) C16 0.033(3) 0.032(3) 0.034(2) -0.001(2) 0.008(2) -0.007(2) C17 0.031(3) 0.045(3) 0.047(3) 0.007(2) 0.002(2) -0.002(2) C18 0.042(3) 0.031(3) 0.042(3) -0.001(2) 0.007(2) 0.003(2) C19 0.037(3) 0.035(3) 0.035(3) -0.003(2) 0.009(2) -0.003(2) C20 0.029(3) 0.045(3) 0.048(3) -0.007(2) 0.006(2) -0.006(2) C21 0.030(3) 0.037(3) 0.050(3) -0.008(2) 0.010(2) 0.002(2) C22 0.051(4) 0.034(3) 0.041(3) 0.007(2) 0.012(3) 0.003(2) N3 0.073(3) 0.046(3) 0.045(2) -0.006(2) 0.010(2) -0.008(2) As1 0.0396(3) 0.0405(3) 0.0486(3) 0.0000(2) 0.0066(3) 0.0075(2) F1 0.101(11) 0.138(12) 0.069(8) 0.043(7) 0.047(7) 0.050(9) F2 0.054(9) 0.126(8) 0.086(9) -0.059(6) -0.006(6) 0.061(6) F3 0.048(2) 0.077(2) 0.140(3) -0.0421(19) -0.019(2) 0.0077(16) F4 0.167(14) 0.083(9) 0.050(6) 0.011(5) 0.031(7) 0.000(7) F5 0.091(9) 0.076(13) 0.089(8) -0.046(8) 0.041(7) 0.032(8) F6 0.056(2) 0.088(2) 0.185(4) -0.031(2) -0.051(2) 0.0309(19) F7 0.049(9) 0.053(5) 0.101(12) -0.058(6) -0.018(7) 0.037(5) F8 0.092(7) 0.089(7) 0.085(10) 0.045(7) -0.001(7) -0.035(5) F9 0.099(13) 0.049(6) 0.115(12) -0.012(6) -0.028(10) 0.027(7) F10 0.090(8) 0.077(8) 0.079(9) 0.013(5) 0.032(6) -0.017(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 N3 2.246(4) 1_656 ? Ag1 N2 2.261(3) . ? Ag1 O3 2.494(2) 3_757 ? Ag1 O2 2.536(3) 3_757 ? C1 O1 1.359(4) . ? C1 C6 1.372(5) . ? C1 C2 1.395(5) . ? C2 C3 1.374(5) . ? C2 H2 0.9500 . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(5) . ? C4 C7 1.445(5) . ? C5 C6 1.373(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N2 1.144(5) . ? O1 C8 1.439(4) . ? C8 C9 1.486(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.433(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O2 C10 1.425(4) . ? O2 Ag1 2.536(3) 3_757 ? C10 C11 1.496(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O3 1.433(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O3 C12 1.430(4) . ? O3 Ag1 2.494(2) 3_757 ? C12 C13 1.498(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O4 1.423(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O4 C14 1.430(4) . ? C14 C15 1.470(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O5 1.447(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O5 C16 1.364(4) . ? C16 C21 1.384(5) . ? C16 C17 1.401(5) . ? C17 C18 1.376(5) . ? C17 H17 0.9500 . ? C18 C19 1.373(5) . ? C18 H18 0.9500 . ? C19 C20 1.391(5) . ? C19 C22 1.431(6) . ? C20 C21 1.370(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 N3 1.148(5) . ? N3 Ag1 2.246(4) 1_454 ? As1 F7 1.598(13) . ? As1 F8 1.645(14) . ? As1 F5 1.654(16) . ? As1 F4 1.664(13) . ? As1 F6 1.695(3) . ? As1 F3 1.700(3) . ? As1 F9 1.71(2) . ? As1 F10 1.716(12) . ? As1 F1 1.725(14) . ? As1 F2 1.847(15) . ? F1 F8 0.715(18) . ? F2 F7 0.51(3) . ? F4 F10 0.770(13) . ? 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 N3 Ag1 N2 109.49(13) 1_656 . ? N3 Ag1 O3 106.89(11) 1_656 3_757 ? N2 Ag1 O3 141.58(10) . 3_757 ? N3 Ag1 O2 110.09(11) 1_656 3_757 ? N2 Ag1 O2 110.80(11) . 3_757 ? O3 Ag1 O2 66.44(9) 3_757 3_757 ? O1 C1 C6 124.5(4) . . ? O1 C1 C2 116.2(4) . . ? C6 C1 C2 119.3(4) . . ? C3 C2 C1 120.9(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 C7 121.6(4) . . ? C5 C4 C7 118.4(4) . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C1 C6 C5 120.5(4) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N2 C7 C4 177.4(5) . . ? C7 N2 Ag1 152.8(3) . . ? C1 O1 C8 117.2(3) . . ? O1 C8 C9 108.0(3) . . ? O1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? O1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O2 C9 C8 109.1(3) . . ? O2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C10 O2 C9 111.3(3) . . ? C10 O2 Ag1 112.5(2) . 3_757 ? C9 O2 Ag1 123.1(2) . 3_757 ? O2 C10 C11 109.2(3) . . ? O2 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? O2 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? O3 C11 C10 108.2(3) . . ? O3 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? O3 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C12 O3 C11 111.4(3) . . ? C12 O3 Ag1 117.6(2) . 3_757 ? C11 O3 Ag1 116.0(2) . 3_757 ? O3 C12 C13 107.9(3) . . ? O3 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? O3 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? O4 C13 C12 107.7(4) . . ? O4 C13 H13A 110.2 . . ? C12 C13 H13A 110.2 . . ? O4 C13 H13B 110.2 . . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C13 O4 C14 115.4(3) . . ? O4 C14 C15 114.5(4) . . ? O4 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? O4 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? O5 C15 C14 108.6(4) . . ? O5 C15 H15A 110.0 . . ? C14 C15 H15A 110.0 . . ? O5 C15 H15B 110.0 . . ? C14 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C16 O5 C15 116.8(3) . . ? O5 C16 C21 124.6(4) . . ? O5 C16 C17 115.4(4) . . ? C21 C16 C17 120.0(4) . . ? C18 C17 C16 119.4(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 C22 120.5(4) . . ? C20 C19 C22 119.7(4) . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C16 119.7(4) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? N3 C22 C19 178.5(5) . . ? C22 N3 Ag1 165.1(4) . 1_454 ? F7 As1 F8 72.6(9) . . ? F7 As1 F5 165.4(12) . . ? F8 As1 F5 93.3(11) . . ? F7 As1 F4 88.2(9) . . ? F8 As1 F4 153.6(5) . . ? F5 As1 F4 103.9(10) . . ? F7 As1 F6 86.5(7) . . ? F8 As1 F6 82.9(5) . . ? F5 As1 F6 87.9(10) . . ? F4 As1 F6 77.8(5) . . ? F7 As1 F3 91.8(7) . . ? F8 As1 F3 97.9(5) . . ? F5 As1 F3 94.0(10) . . ? F4 As1 F3 100.7(5) . . ? F6 As1 F3 177.81(16) . . ? F7 As1 F9 177.9(11) . . ? F8 As1 F9 105.7(11) . . ? F4 As1 F9 93.0(10) . . ? F6 As1 F9 92.0(9) . . ? F3 As1 F9 89.7(9) . . ? F7 As1 F10 106.6(8) . . ? F8 As1 F10 179.0(8) . . ? F5 As1 F10 87.5(11) . . ? F6 As1 F10 97.6(5) . . ? F3 As1 F10 81.5(5) . . ? F9 As1 F10 75.1(10) . . ? F7 As1 F1 89.6(9) . . ? F5 As1 F1 78.2(11) . . ? F4 As1 F1 177.7(6) . . ? F6 As1 F1 101.3(5) . . ? F3 As1 F1 80.0(5) . . ? F9 As1 F1 89.2(10) . . ? F10 As1 F1 155.7(5) . . ? F8 As1 F2 86.9(9) . . ? F5 As1 F2 179.5(13) . . ? F4 As1 F2 76.1(9) . . ? F6 As1 F2 92.6(7) . . ? F3 As1 F2 85.5(7) . . ? F9 As1 F2 167.0(12) . . ? F10 As1 F2 92.3(8) . . ? F1 As1 F2 101.8(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.672 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.122 # Attachment 'New CIF for 4-AgSbF6.cif' data_4-AgSbF6 _database_code_depnum_ccdc_archive 'CCDC 624587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Ag N2 O5, F6 Sb' _chemical_formula_sum 'C22 H24 Ag F6 N2 O5 Sb' _chemical_formula_weight 740.05 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.9640(1) _cell_length_b 25.7170(4) _cell_length_c 8.6320(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.0780(6) _cell_angle_gamma 90.00 _cell_volume 2635.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7625 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7822 _exptl_absorpt_correction_T_max 0.8370 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 14336 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7709 _reflns_number_gt 4935 _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^)+(0.0660P)^2^+0.1608P] 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 7709 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 1.26024(3) -0.163988(12) 1.15355(4) 0.04065(11) Uani 1 1 d . . . C1 C 1.0262(3) 0.08026(15) 0.7967(4) 0.0311(8) Uani 1 1 d . . . C2 C 0.9857(3) 0.03725(15) 0.7090(4) 0.0352(9) Uani 1 1 d . . . H2 H 0.9305 0.0418 0.6211 0.042 Uiso 1 1 calc R . . C3 C 1.0251(3) -0.01185(15) 0.7490(4) 0.0374(9) Uani 1 1 d . . . H3 H 0.9971 -0.0410 0.6889 0.045 Uiso 1 1 calc R . . C4 C 1.1059(3) -0.01858(14) 0.8774(4) 0.0313(8) Uani 1 1 d . . . C5 C 1.1454(3) 0.02438(15) 0.9663(4) 0.0336(8) Uani 1 1 d . . . H5 H 1.1995 0.0196 1.0555 0.040 Uiso 1 1 calc R . . C6 C 1.1068(3) 0.07396(14) 0.9258(4) 0.0316(8) Uani 1 1 d . . . H6 H 1.1349 0.1032 0.9855 0.038 Uiso 1 1 calc R . . C7 C 1.1488(3) -0.06929(16) 0.9245(4) 0.0357(9) Uani 1 1 d . . . N2 N 1.1871(3) -0.10823(13) 0.9672(4) 0.0423(8) Uani 1 1 d . . . O1 O 0.9814(2) 0.12680(10) 0.7493(3) 0.0344(6) Uani 1 1 d . . . C8 C 1.0395(3) 0.17279(15) 0.8117(5) 0.0388(9) Uani 1 1 d . . . H8A H 1.1203 0.1707 0.7979 0.047 Uiso 1 1 calc R . . H8B H 1.0333 0.1759 0.9247 0.047 Uiso 1 1 calc R . . C9 C 0.9863(3) 0.21907(15) 0.7256(5) 0.0394(9) Uani 1 1 d . . . H9A H 1.0385 0.2491 0.7376 0.047 Uiso 1 1 calc R . . H9B H 0.9696 0.2110 0.6130 0.047 Uiso 1 1 calc R . . O2 O 0.8840(2) 0.23163(10) 0.7887(3) 0.0345(6) Uani 1 1 d . . . C10 C 0.8336(3) 0.27701(14) 0.7188(4) 0.0334(8) Uani 1 1 d . . . H10A H 0.8031 0.2697 0.6090 0.040 Uiso 1 1 calc R . . H10B H 0.8906 0.3049 0.7191 0.040 Uiso 1 1 calc R . . C11 C 0.7404(3) 0.29440(15) 0.8078(4) 0.0348(9) Uani 1 1 d . . . H11A H 0.7712 0.3031 0.9164 0.042 Uiso 1 1 calc R . . H11B H 0.7041 0.3259 0.7586 0.042 Uiso 1 1 calc R . . O3 O 0.6598(2) 0.25371(10) 0.8077(3) 0.0335(6) Uani 1 1 d . . . C12 C 0.5685(4) 0.26706(15) 0.8931(5) 0.0411(10) Uani 1 1 d . . . H12A H 0.5268 0.2972 0.8437 0.049 Uiso 1 1 calc R . . H12B H 0.5979 0.2766 1.0016 0.049 Uiso 1 1 calc R . . C13 C 0.4917(4) 0.22096(18) 0.8930(5) 0.0496(11) Uani 1 1 d . . . H13A H 0.4260 0.2295 0.9475 0.059 Uiso 1 1 calc R . . H13B H 0.4641 0.2106 0.7845 0.059 Uiso 1 1 calc R . . O4 O 0.5553(2) 0.17951(11) 0.9720(3) 0.0429(7) Uani 1 1 d . . . C14 C 0.4871(4) 0.14205(17) 1.0402(5) 0.0478(11) Uani 1 1 d . . . H14A H 0.4329 0.1607 1.0979 0.057 Uiso 1 1 calc R . . H14B H 0.5362 0.1209 1.1166 0.057 Uiso 1 1 calc R . . C15 C 0.4235(4) 0.10661(17) 0.9248(5) 0.0444(10) Uani 1 1 d . . . H15A H 0.3625 0.0891 0.9726 0.053 Uiso 1 1 calc R . . H15B H 0.3892 0.1267 0.8332 0.053 Uiso 1 1 calc R . . O5 O 0.5008(2) 0.06872(11) 0.8773(3) 0.0435(7) Uani 1 1 d . . . C16 C 0.4572(3) 0.03095(15) 0.7768(4) 0.0322(8) Uani 1 1 d . . . C17 C 0.5318(4) -0.00835(16) 0.7455(4) 0.0394(9) Uani 1 1 d . . . H17 H 0.6074 -0.0077 0.7944 0.047 Uiso 1 1 calc R . . C18 C 0.4964(4) -0.04782(16) 0.6446(5) 0.0393(9) Uani 1 1 d . . . H18 H 0.5477 -0.0741 0.6220 0.047 Uiso 1 1 calc R . . C19 C 0.3855(4) -0.04927(16) 0.5754(4) 0.0373(9) Uani 1 1 d . . . C20 C 0.3115(4) -0.00977(17) 0.6057(5) 0.0411(10) Uani 1 1 d . . . H20 H 0.2361 -0.0102 0.5562 0.049 Uiso 1 1 calc R . . C21 C 0.3471(3) 0.03003(16) 0.7071(4) 0.0383(9) Uani 1 1 d . . . H21 H 0.2962 0.0566 0.7288 0.046 Uiso 1 1 calc R . . C22 C 0.3488(4) -0.08887(17) 0.4647(5) 0.0416(10) Uani 1 1 d . . . N3 N 0.3187(3) -0.12066(14) 0.3759(4) 0.0503(9) Uani 1 1 d . . . Sb1 Sb 0.21294(2) 0.149535(11) 0.37835(3) 0.03992(11) Uani 1 1 d . . . F1 F 0.1895(5) 0.1236(2) 0.5760(7) 0.0700(7) Uani 0.50 1 d P . . F2 F 0.2645(6) 0.0954(3) 0.2538(7) 0.0700(7) Uani 0.50 1 d P . . F3 F 0.3586(3) 0.15110(13) 0.4792(5) 0.1012(14) Uani 1 1 d . . . F4 F 0.2301(6) 0.1736(3) 0.1835(7) 0.0700(7) Uani 0.50 1 d P . . F5 F 0.1656(7) 0.2027(3) 0.4939(8) 0.0700(7) Uani 0.50 1 d P . . F6 F 0.0708(3) 0.14595(15) 0.2697(6) 0.133(2) Uani 1 1 d . . . F7 F 0.2359(6) 0.0813(3) 0.3106(7) 0.0700(7) Uani 0.50 1 d P . . F8 F 0.1556(5) 0.1014(3) 0.5017(7) 0.0700(7) Uani 0.50 1 d P . . F9 F 0.1843(7) 0.2166(3) 0.4493(8) 0.0700(7) Uani 0.50 1 d P . . F10 F 0.2784(6) 0.1975(3) 0.2477(7) 0.0700(7) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0549(2) 0.02604(17) 0.04059(19) 0.00008(12) 0.00439(15) 0.00193(14) C1 0.0258(19) 0.029(2) 0.040(2) 0.0059(16) 0.0087(16) 0.0006(15) C2 0.037(2) 0.033(2) 0.034(2) 0.0022(16) -0.0016(17) -0.0028(17) C3 0.042(2) 0.032(2) 0.038(2) -0.0032(17) 0.0036(17) 0.0011(18) C4 0.034(2) 0.0225(18) 0.039(2) 0.0032(15) 0.0112(16) -0.0002(15) C5 0.030(2) 0.036(2) 0.0341(19) 0.0024(16) 0.0003(15) 0.0006(17) C6 0.030(2) 0.0258(19) 0.039(2) -0.0078(16) 0.0040(16) -0.0007(15) C7 0.038(2) 0.036(2) 0.0335(19) 0.0001(17) 0.0070(17) -0.0006(18) N2 0.053(2) 0.0286(18) 0.0451(19) 0.0023(16) 0.0050(17) 0.0087(16) O1 0.0313(15) 0.0252(14) 0.0456(15) 0.0020(12) -0.0001(11) 0.0012(11) C8 0.034(2) 0.028(2) 0.054(2) -0.0022(18) 0.0048(18) 0.0012(17) C9 0.035(2) 0.031(2) 0.054(2) 0.0032(18) 0.0119(19) -0.0018(17) O2 0.0353(15) 0.0252(14) 0.0444(15) 0.0053(12) 0.0102(12) 0.0060(11) C10 0.038(2) 0.0255(19) 0.0369(19) 0.0067(16) 0.0056(16) 0.0007(16) C11 0.038(2) 0.0245(19) 0.041(2) 0.0024(16) 0.0017(17) -0.0012(16) O3 0.0371(16) 0.0270(14) 0.0376(14) 0.0005(11) 0.0085(12) 0.0007(11) C12 0.040(2) 0.032(2) 0.052(2) 0.0051(19) 0.0125(19) 0.0072(18) C13 0.035(2) 0.053(3) 0.061(3) 0.008(2) 0.006(2) 0.000(2) O4 0.0454(18) 0.0311(15) 0.0534(17) 0.0031(13) 0.0108(14) -0.0071(13) C14 0.054(3) 0.046(3) 0.045(2) -0.005(2) 0.012(2) -0.016(2) C15 0.041(2) 0.041(2) 0.053(2) -0.013(2) 0.0134(19) -0.0119(19) O5 0.0374(16) 0.0440(18) 0.0482(17) -0.0078(13) 0.0013(13) -0.0068(13) C16 0.036(2) 0.032(2) 0.0294(18) 0.0019(15) 0.0051(16) -0.0058(16) C17 0.037(2) 0.039(2) 0.042(2) 0.0052(18) 0.0019(17) 0.0015(18) C18 0.043(3) 0.033(2) 0.043(2) 0.0034(18) 0.0077(18) 0.0038(18) C19 0.045(3) 0.035(2) 0.0327(19) -0.0010(17) 0.0104(18) -0.0072(19) C20 0.035(2) 0.041(2) 0.046(2) -0.0043(19) 0.0018(18) -0.0060(18) C21 0.032(2) 0.041(2) 0.043(2) -0.0076(18) 0.0107(17) 0.0024(17) C22 0.052(3) 0.035(2) 0.039(2) 0.0028(19) 0.0108(19) -0.003(2) N3 0.068(3) 0.037(2) 0.047(2) -0.0069(17) 0.0114(18) -0.0080(19) Sb1 0.03690(18) 0.03764(18) 0.04483(18) -0.00184(12) 0.00346(12) 0.00470(12) F1 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F2 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F3 0.050(2) 0.075(2) 0.170(4) -0.049(2) -0.025(2) 0.0074(16) F4 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F5 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F6 0.068(3) 0.088(3) 0.220(5) -0.052(3) -0.069(3) 0.041(2) F7 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F8 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F9 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) F10 0.0832(19) 0.0613(19) 0.066(2) -0.0028(11) 0.0096(12) 0.0075(14) _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 2.250(3) . ? Ag1 N3 2.255(4) 1_656 ? Ag1 O3 2.505(3) 3_757 ? Ag1 O2 2.543(3) 3_757 ? C1 O1 1.354(4) . ? C1 C6 1.390(5) . ? C1 C2 1.393(5) . ? C2 C3 1.377(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 C7 1.442(5) . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N2 1.143(5) . ? O1 C8 1.442(5) . ? C8 C9 1.503(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.436(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O2 C10 1.415(4) . ? O2 Ag1 2.543(3) 3_757 ? C10 C11 1.498(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O3 1.423(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O3 C12 1.432(5) . ? O3 Ag1 2.505(3) 3_757 ? C12 C13 1.500(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O4 1.432(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O4 C14 1.435(5) . ? C14 C15 1.488(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O5 1.438(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O5 C16 1.363(4) . ? C16 C21 1.379(5) . ? C16 C17 1.397(6) . ? C17 C18 1.370(6) . ? C17 H17 0.9500 . ? C18 C19 1.387(6) . ? C18 H18 0.9500 . ? C19 C20 1.393(6) . ? C19 C22 1.428(6) . ? C20 C21 1.380(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 N3 1.147(5) . ? N3 Ag1 2.255(4) 1_454 ? Sb1 F8 1.821(6) . ? Sb1 F5 1.823(8) . ? Sb1 F4 1.827(6) . ? Sb1 F6 1.840(3) . ? Sb1 F3 1.850(3) . ? Sb1 F9 1.875(8) . ? Sb1 F7 1.881(7) . ? Sb1 F1 1.885(6) . ? Sb1 F10 1.904(6) . ? Sb1 F2 1.907(7) . ? 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 N3 110.26(13) . 1_656 ? N2 Ag1 O3 142.29(10) . 3_757 ? N3 Ag1 O3 105.55(11) 1_656 3_757 ? N2 Ag1 O2 111.27(11) . 3_757 ? N3 Ag1 O2 108.55(11) 1_656 3_757 ? O3 Ag1 O2 66.48(8) 3_757 3_757 ? O1 C1 C6 123.7(4) . . ? O1 C1 C2 116.1(3) . . ? C6 C1 C2 120.2(4) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 C7 121.8(4) . . ? C5 C4 C7 118.5(3) . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.1(4) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? N2 C7 C4 176.4(4) . . ? C7 N2 Ag1 153.3(3) . . ? C1 O1 C8 117.2(3) . . ? O1 C8 C9 108.0(3) . . ? O1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? O1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O2 C9 C8 108.6(3) . . ? O2 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? O2 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C10 O2 C9 111.2(3) . . ? C10 O2 Ag1 112.6(2) . 3_757 ? C9 O2 Ag1 123.4(2) . 3_757 ? O2 C10 C11 109.4(3) . . ? O2 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? O2 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? O3 C11 C10 109.1(3) . . ? O3 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? O3 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 O3 C12 112.5(3) . . ? C11 O3 Ag1 115.4(2) . 3_757 ? C12 O3 Ag1 117.1(2) . 3_757 ? O3 C12 C13 108.4(3) . . ? O3 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? O3 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? O4 C13 C12 107.4(3) . . ? O4 C13 H13A 110.2 . . ? C12 C13 H13A 110.2 . . ? O4 C13 H13B 110.2 . . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C13 O4 C14 113.5(3) . . ? O4 C14 C15 114.0(4) . . ? O4 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? O4 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? O5 C15 C14 108.2(4) . . ? O5 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? O5 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? C16 O5 C15 117.1(3) . . ? O5 C16 C21 124.1(4) . . ? O5 C16 C17 115.8(4) . . ? C21 C16 C17 120.1(4) . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 C22 120.4(4) . . ? C20 C19 C22 119.7(4) . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C16 C21 C20 119.6(4) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? N3 C22 C19 179.7(5) . . ? C22 N3 Ag1 163.6(3) . 1_454 ? F8 Sb1 F5 91.5(3) . . ? F8 Sb1 F4 149.5(3) . . ? F5 Sb1 F4 109.0(3) . . ? F8 Sb1 F6 82.7(3) . . ? F5 Sb1 F6 89.2(3) . . ? F4 Sb1 F6 75.5(3) . . ? F8 Sb1 F3 98.1(2) . . ? F5 Sb1 F3 93.7(3) . . ? F4 Sb1 F3 102.7(3) . . ? F6 Sb1 F3 176.93(18) . . ? F8 Sb1 F9 109.7(3) . . ? F5 Sb1 F9 18.2(3) . . ? F4 Sb1 F9 92.0(3) . . ? F6 Sb1 F9 91.0(3) . . ? F3 Sb1 F9 91.5(3) . . ? F8 Sb1 F7 68.1(3) . . ? F5 Sb1 F7 159.6(3) . . ? F4 Sb1 F7 89.6(3) . . ? F6 Sb1 F7 87.5(2) . . ? F3 Sb1 F7 90.1(2) . . ? F9 Sb1 F7 177.5(3) . . ? F8 Sb1 F1 28.5(2) . . ? F5 Sb1 F1 71.3(3) . . ? F4 Sb1 F1 177.7(3) . . ? F6 Sb1 F1 102.3(3) . . ? F3 Sb1 F1 79.6(3) . . ? F9 Sb1 F1 88.6(3) . . ? F7 Sb1 F1 89.7(3) . . ? F8 Sb1 F10 177.2(3) . . ? F5 Sb1 F10 90.9(3) . . ? F4 Sb1 F10 30.0(2) . . ? F6 Sb1 F10 98.7(3) . . ? F3 Sb1 F10 80.3(2) . . ? F9 Sb1 F10 72.7(3) . . ? F7 Sb1 F10 109.5(3) . . ? F1 Sb1 F10 152.1(3) . . ? F8 Sb1 F2 90.3(3) . . ? F5 Sb1 F2 178.3(3) . . ? F4 Sb1 F2 69.4(3) . . ? F6 Sb1 F2 91.1(2) . . ? F3 Sb1 F2 86.0(2) . . ? F9 Sb1 F2 160.0(3) . . ? F7 Sb1 F2 22.2(2) . . ? F1 Sb1 F2 110.3(3) . . ? F10 Sb1 F2 87.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.247 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.124