# These structures are included in a paper submitted to Organometallics # Title: Synthesis and Characterization of Silver Hexafluoroacetonate Complexes # Authors: William J. Evans, Dimitrios G. Giarikos, Daniel Jossel, and Joseph W. Ziller # Contact author: William J. Evans, UC Irvine, Irvine, CA 92697-2025 # email: wevans@uci.edu # CCDC DEPOSIT, DEPOSITION NUMBERS dg57(212248), dg58(212249), dg60(212250), dg61(212251) data_dg57 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H20 Ag4 F24 O8' _chemical_formula_weight 1443.98 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.271(3) _cell_length_b 12.5725(10) _cell_length_c 16.4444(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.7670(10) _cell_angle_gamma 90.00 _cell_volume 8528.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5997 _exptl_absorpt_correction_T_max 0.7984 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 43984 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10336 _reflns_number_gt 8371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0328P)^2^+26.0663P] 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 10336 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.140477(6) 0.39500(2) 0.240005(14) 0.02969(6) Uani 1 1 d . . . Ag2 Ag 0.114820(6) 0.413597(19) 0.037070(14) 0.02930(6) Uani 1 1 d . . . Ag3 Ag 0.125222(6) 0.125961(19) 0.012255(15) 0.02999(6) Uani 1 1 d . . . Ag4 Ag 0.121218(6) 0.10662(2) 0.216297(16) 0.03272(7) Uani 1 1 d . . . O1 O 0.09415(5) 0.47801(18) 0.16484(13) 0.0300(5) Uani 1 1 d . . . O2 O 0.09661(5) 0.27164(18) 0.24511(14) 0.0344(5) Uani 1 1 d . . . O3 O 0.08567(5) 0.04062(18) 0.11104(13) 0.0317(5) Uani 1 1 d . . . O4 O 0.08368(5) 0.25494(18) 0.04596(14) 0.0321(5) Uani 1 1 d . . . O5 O 0.15974(5) 0.03979(18) 0.11091(13) 0.0318(5) Uani 1 1 d . . . O6 O 0.16660(5) 0.22827(18) 0.21347(14) 0.0325(5) Uani 1 1 d . . . O7 O 0.15579(5) 0.28347(18) 0.01114(14) 0.0324(5) Uani 1 1 d . . . O8 O 0.16248(5) 0.46720(18) 0.11674(13) 0.0304(5) Uani 1 1 d . . . C1 C 0.04489(8) 0.5712(3) 0.1721(2) 0.0366(8) Uani 1 1 d . . . C2 C 0.06599(7) 0.4719(3) 0.19019(18) 0.0280(6) Uani 1 1 d . . . C3 C 0.05179(7) 0.3912(3) 0.2349(2) 0.0312(7) Uani 1 1 d . . . H3A H 0.0299 0.3996 0.2496 0.037 Uiso 1 1 calc R . . C4 C 0.06795(7) 0.2988(3) 0.25926(18) 0.0290(6) Uani 1 1 d . . . C5 C 0.04993(8) 0.2203(3) 0.3125(2) 0.0358(7) Uani 1 1 d . . . C6 C 0.03592(9) -0.0499(3) 0.1132(2) 0.0428(8) Uani 1 1 d . . . C7 C 0.05577(7) 0.0512(3) 0.09802(18) 0.0290(6) Uani 1 1 d . . . C8 C 0.03872(7) 0.1394(3) 0.06731(19) 0.0310(7) Uani 1 1 d . . . H8A H 0.0157 0.1358 0.0634 0.037 Uiso 1 1 calc R . . C9 C 0.05391(7) 0.2324(3) 0.04217(18) 0.0285(6) Uani 1 1 d . . . C10 C 0.03222(8) 0.3147(3) -0.0019(2) 0.0362(7) Uani 1 1 d . . . C11 C 0.20740(8) -0.0567(3) 0.0893(2) 0.0381(8) Uani 1 1 d . . . C12 C 0.18978(7) 0.0394(3) 0.12514(18) 0.0291(6) Uani 1 1 d . . . C13 C 0.20849(8) 0.1097(3) 0.1726(2) 0.0313(7) Uani 1 1 d . . . H13A H 0.2312 0.0976 0.1775 0.038 Uiso 1 1 calc R . . C14 C 0.19565(7) 0.1966(3) 0.21335(19) 0.0300(7) Uani 1 1 d . . . C15 C 0.21929(8) 0.2612(3) 0.2674(2) 0.0372(8) Uani 1 1 d . . . C16 C 0.20117(8) 0.2396(3) -0.0650(2) 0.0325(7) Uani 1 1 d . . . C17 C 0.18488(7) 0.3077(2) -0.00059(19) 0.0281(6) Uani 1 1 d . . . C18 C 0.20322(7) 0.3886(3) 0.0359(2) 0.0310(7) Uani 1 1 d . . . H18A H 0.2253 0.3952 0.0223 0.037 Uiso 1 1 calc R . . C19 C 0.19073(7) 0.4608(2) 0.09166(19) 0.0288(6) Uani 1 1 d . . . C20 C 0.21407(8) 0.5476(3) 0.1244(2) 0.0389(8) Uani 1 1 d . . . C21 C 0.11292(10) -0.0225(3) -0.0838(2) 0.0444(9) Uani 1 1 d . . . H21A H 0.1100 -0.0685 -0.0388 0.053 Uiso 1 1 calc R . . C22 C 0.08955(10) 0.0527(3) -0.1053(2) 0.0439(9) Uani 1 1 d . . . H22A H 0.0705 0.0582 -0.0744 0.053 Uiso 1 1 calc R . . C23 C 0.09353(10) 0.1202(3) -0.1716(2) 0.0432(9) Uani 1 1 d . . . H23A H 0.0774 0.1717 -0.1849 0.052 Uiso 1 1 calc R . . C24 C 0.12082(9) 0.1131(3) -0.2183(2) 0.0379(8) Uani 1 1 d . . . C25 C 0.14455(9) 0.0382(3) -0.1954(2) 0.0369(8) Uani 1 1 d . . . H25A H 0.1637 0.0333 -0.2258 0.044 Uiso 1 1 calc R . . C26 C 0.14078(10) -0.0291(3) -0.1294(2) 0.0432(9) Uani 1 1 d . . . H26A H 0.1572 -0.0796 -0.1154 0.052 Uiso 1 1 calc R . . C27 C 0.12540(12) 0.1847(3) -0.2907(2) 0.0532(10) Uani 1 1 d . . . H27A H 0.1066 0.2319 -0.2975 0.080 Uiso 1 1 calc R . . H27B H 0.1275 0.1413 -0.3398 0.080 Uiso 1 1 calc R . . H27C H 0.1450 0.2275 -0.2819 0.080 Uiso 1 1 calc R . . C28 C 0.10239(9) 0.5544(3) -0.06311(19) 0.0358(7) Uani 1 1 d . . . H28A H 0.0826 0.5709 -0.0377 0.043 Uiso 1 1 calc R . . C29 C 0.10326(10) 0.4713(3) -0.1193(2) 0.0427(9) Uani 1 1 d . . . H29A H 0.0842 0.4313 -0.1316 0.051 Uiso 1 1 calc R . . C30 C 0.13197(12) 0.4470(3) -0.1571(2) 0.0507(10) Uani 1 1 d . . . H30A H 0.1327 0.3902 -0.1951 0.061 Uiso 1 1 calc R . . C31 C 0.15945(10) 0.5058(3) -0.1391(2) 0.0496(10) Uani 1 1 d . . . H31A H 0.1791 0.4895 -0.1649 0.060 Uiso 1 1 calc R . . C32 C 0.15850(10) 0.5887(3) -0.0833(2) 0.0468(9) Uani 1 1 d . . . H32A H 0.1776 0.6291 -0.0719 0.056 Uiso 1 1 calc R . . C33 C 0.13023(9) 0.6137(3) -0.0439(2) 0.0389(8) Uani 1 1 d . . . C34 C 0.12917(13) 0.7003(3) 0.0192(3) 0.0641(12) Uani 1 1 d . . . H34A H 0.1505 0.7339 0.0250 0.096 Uiso 1 1 calc R . . H34B H 0.1232 0.6696 0.0715 0.096 Uiso 1 1 calc R . . H34C H 0.1130 0.7537 0.0023 0.096 Uiso 1 1 calc R . . F1 F 0.04761(7) 0.63964(19) 0.23399(15) 0.0613(7) Uani 1 1 d . . . F2 F 0.01345(5) 0.5482(2) 0.16255(16) 0.0558(6) Uani 1 1 d . . . F3 F 0.05363(6) 0.62165(19) 0.10581(14) 0.0544(6) Uani 1 1 d . . . F4 F 0.05116(6) 0.12188(18) 0.28221(15) 0.0562(6) Uani 1 1 d . . . F5 F 0.01885(5) 0.2440(2) 0.32207(16) 0.0625(7) Uani 1 1 d . . . F6 F 0.06369(6) 0.21578(19) 0.38688(13) 0.0536(6) Uani 1 1 d . . . F7 F 0.00423(6) -0.0358(2) 0.1098(2) 0.0807(9) Uani 1 1 d . . . F8 F 0.04150(9) -0.1197(2) 0.0548(2) 0.0962(11) Uani 1 1 d . . . F9 F 0.04369(8) -0.0947(2) 0.18203(19) 0.0892(11) Uani 1 1 d . . . F10 F 0.03499(7) 0.3029(2) -0.08221(14) 0.0636(7) Uani 1 1 d . . . F11 F 0.00117(5) 0.3071(2) 0.01369(17) 0.0630(7) Uani 1 1 d . . . F12 F 0.04147(6) 0.41450(17) 0.01574(16) 0.0521(6) Uani 1 1 d . . . F13 F 0.23902(6) -0.0404(2) 0.08054(18) 0.0721(8) Uani 1 1 d . . . F14 F 0.20492(7) -0.1395(2) 0.13796(17) 0.0709(8) Uani 1 1 d . . . F15 F 0.19530(7) -0.0847(2) 0.01767(15) 0.0658(7) Uani 1 1 d . . . F16 F 0.21497(6) 0.2364(2) 0.34549(13) 0.0576(6) Uani 1 1 d . . . F17 F 0.25026(5) 0.2448(2) 0.25223(15) 0.0579(7) Uani 1 1 d . . . F18 F 0.21379(5) 0.36575(17) 0.26034(15) 0.0501(6) Uani 1 1 d . . . F19 F 0.18521(6) 0.2472(2) -0.13627(13) 0.0536(6) Uani 1 1 d . . . F20 F 0.23169(5) 0.2658(2) -0.07823(15) 0.0578(7) Uani 1 1 d . . . F21 F 0.20128(7) 0.13728(18) -0.04470(15) 0.0619(7) Uani 1 1 d . . . F22 F 0.21441(7) 0.62929(19) 0.07369(17) 0.0675(8) Uani 1 1 d . . . F23 F 0.20524(6) 0.5837(2) 0.19618(15) 0.0646(7) Uani 1 1 d . . . F24 F 0.24457(5) 0.5145(2) 0.13349(17) 0.0637(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02606(12) 0.03214(13) 0.03094(12) -0.00073(9) 0.00212(9) 0.00260(9) Ag2 0.02758(12) 0.02849(13) 0.03197(13) 0.00114(9) 0.00314(9) -0.00065(9) Ag3 0.02897(12) 0.02790(13) 0.03304(13) 0.00138(9) 0.00020(9) -0.00042(9) Ag4 0.02878(12) 0.03081(13) 0.03869(14) -0.00357(10) 0.00302(10) -0.00144(10) O1 0.0247(10) 0.0341(12) 0.0315(11) 0.0017(9) 0.0051(9) 0.0019(9) O2 0.0244(11) 0.0324(13) 0.0466(13) 0.0027(10) 0.0034(9) 0.0058(9) O3 0.0279(11) 0.0338(13) 0.0331(12) -0.0002(9) -0.0034(9) -0.0006(9) O4 0.0223(10) 0.0301(12) 0.0438(13) -0.0005(10) 0.0012(9) -0.0032(9) O5 0.0265(11) 0.0349(13) 0.0338(12) 0.0041(10) -0.0002(9) 0.0016(9) O6 0.0221(10) 0.0288(12) 0.0467(13) -0.0013(10) 0.0030(9) 0.0041(9) O7 0.0218(10) 0.0306(12) 0.0450(13) -0.0004(10) 0.0052(9) -0.0024(9) O8 0.0258(11) 0.0328(12) 0.0330(11) -0.0018(9) 0.0062(9) -0.0014(9) C1 0.0342(17) 0.0387(19) 0.0373(18) 0.0073(15) 0.0052(14) 0.0093(15) C2 0.0226(14) 0.0346(17) 0.0268(15) -0.0007(12) 0.0008(12) 0.0063(12) C3 0.0203(14) 0.0372(18) 0.0364(17) 0.0038(14) 0.0050(12) 0.0042(13) C4 0.0252(15) 0.0330(17) 0.0287(15) -0.0004(13) 0.0016(12) 0.0009(13) C5 0.0322(17) 0.039(2) 0.0361(18) 0.0068(15) 0.0036(14) 0.0037(14) C6 0.041(2) 0.039(2) 0.048(2) 0.0071(17) -0.0046(16) -0.0097(16) C7 0.0291(15) 0.0324(17) 0.0256(15) -0.0012(12) 0.0004(12) -0.0051(13) C8 0.0211(14) 0.0373(18) 0.0345(17) -0.0006(14) -0.0007(12) -0.0056(13) C9 0.0248(14) 0.0322(17) 0.0285(15) -0.0011(12) 0.0009(12) 0.0016(12) C10 0.0304(16) 0.0375(19) 0.0407(18) 0.0022(15) -0.0001(14) -0.0004(14) C11 0.0351(18) 0.0359(19) 0.0431(19) -0.0025(15) -0.0005(15) 0.0047(15) C12 0.0281(15) 0.0315(17) 0.0279(15) 0.0045(13) 0.0036(12) 0.0044(13) C13 0.0230(14) 0.0344(18) 0.0364(17) 0.0004(13) -0.0012(12) 0.0075(13) C14 0.0247(14) 0.0317(17) 0.0334(16) 0.0035(13) -0.0007(12) 0.0016(13) C15 0.0297(16) 0.0380(19) 0.044(2) -0.0059(15) -0.0033(14) 0.0074(14) C16 0.0285(15) 0.0333(18) 0.0360(17) -0.0005(14) 0.0044(13) 0.0004(13) C17 0.0252(14) 0.0281(16) 0.0310(15) 0.0041(12) 0.0027(12) 0.0026(12) C18 0.0220(14) 0.0315(17) 0.0396(17) -0.0011(13) 0.0053(13) -0.0038(12) C19 0.0271(15) 0.0271(16) 0.0323(16) 0.0009(12) 0.0015(12) -0.0037(12) C20 0.0350(18) 0.0364(19) 0.045(2) -0.0063(16) 0.0038(15) -0.0091(15) C21 0.071(3) 0.034(2) 0.0279(17) -0.0028(14) -0.0012(17) -0.0097(18) C22 0.049(2) 0.049(2) 0.0335(18) -0.0120(16) 0.0047(16) -0.0094(18) C23 0.048(2) 0.045(2) 0.0360(19) -0.0116(16) -0.0036(16) 0.0069(17) C24 0.056(2) 0.0305(18) 0.0269(16) -0.0058(13) -0.0022(15) -0.0017(16) C25 0.0415(19) 0.0387(19) 0.0303(17) -0.0093(14) -0.0010(14) -0.0041(15) C26 0.060(2) 0.035(2) 0.0341(18) -0.0055(15) -0.0117(17) 0.0024(17) C27 0.085(3) 0.041(2) 0.0344(19) 0.0006(16) 0.002(2) -0.002(2) C28 0.0431(19) 0.0361(18) 0.0284(16) 0.0112(14) 0.0047(14) 0.0044(15) C29 0.055(2) 0.037(2) 0.0351(18) 0.0067(15) -0.0106(16) -0.0043(17) C30 0.083(3) 0.041(2) 0.0286(18) -0.0017(16) -0.0007(19) 0.015(2) C31 0.055(2) 0.060(3) 0.0351(19) 0.0193(18) 0.0134(17) 0.020(2) C32 0.044(2) 0.052(2) 0.045(2) 0.0200(18) 0.0026(17) -0.0063(18) C33 0.053(2) 0.0331(19) 0.0307(17) 0.0094(14) 0.0018(15) -0.0009(16) C34 0.099(4) 0.040(2) 0.052(3) -0.0059(19) -0.004(2) -0.002(2) F1 0.0841(18) 0.0432(14) 0.0564(14) -0.0095(11) -0.0018(13) 0.0248(13) F2 0.0278(10) 0.0607(15) 0.0788(16) 0.0222(13) 0.0017(10) 0.0154(10) F3 0.0547(14) 0.0564(15) 0.0527(13) 0.0269(11) 0.0120(11) 0.0173(11) F4 0.0741(17) 0.0385(13) 0.0566(14) 0.0031(10) 0.0123(12) -0.0165(11) F5 0.0351(11) 0.0733(17) 0.0802(17) 0.0358(14) 0.0214(11) 0.0055(12) F6 0.0686(15) 0.0569(15) 0.0349(11) 0.0110(10) -0.0026(10) -0.0013(12) F7 0.0390(13) 0.0677(18) 0.135(3) 0.0368(18) 0.0010(15) -0.0212(12) F8 0.122(3) 0.0563(18) 0.112(3) -0.0330(17) 0.027(2) -0.0430(18) F9 0.097(2) 0.084(2) 0.084(2) 0.0551(17) -0.0297(18) -0.0407(17) F10 0.0813(18) 0.0712(17) 0.0375(12) 0.0078(12) -0.0121(12) 0.0179(14) F11 0.0252(10) 0.0660(16) 0.0978(19) 0.0312(14) -0.0007(11) 0.0072(10) F12 0.0485(13) 0.0326(12) 0.0746(16) 0.0041(11) -0.0101(12) 0.0037(10) F13 0.0380(13) 0.0726(18) 0.107(2) -0.0421(16) 0.0168(13) 0.0075(12) F14 0.097(2) 0.0415(14) 0.0751(18) 0.0122(13) 0.0115(15) 0.0274(14) F15 0.0780(18) 0.0648(17) 0.0535(15) -0.0273(12) -0.0167(13) 0.0212(14) F16 0.0705(16) 0.0649(16) 0.0369(12) -0.0056(11) -0.0079(11) 0.0054(13) F17 0.0239(9) 0.0733(17) 0.0759(16) -0.0331(13) -0.0077(10) 0.0043(10) F18 0.0437(12) 0.0354(12) 0.0704(15) -0.0075(11) -0.0132(11) -0.0013(9) F19 0.0572(13) 0.0637(15) 0.0393(12) -0.0144(11) -0.0079(10) 0.0134(12) F20 0.0346(11) 0.0785(18) 0.0614(14) -0.0279(13) 0.0187(10) -0.0075(11) F21 0.0885(19) 0.0324(12) 0.0663(16) 0.0034(11) 0.0286(14) 0.0181(12) F22 0.087(2) 0.0421(14) 0.0727(17) 0.0079(12) -0.0097(15) -0.0297(13) F23 0.0659(16) 0.0702(17) 0.0585(15) -0.0331(13) 0.0137(12) -0.0271(13) F24 0.0352(12) 0.0616(16) 0.094(2) -0.0235(14) -0.0067(12) -0.0116(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O2 2.388(2) . ? Ag1 O6 2.403(2) . ? Ag1 O8 2.423(2) . ? Ag1 C31 2.455(4) 6_566 ? Ag1 O1 2.475(2) . ? Ag1 C30 2.640(4) 6_566 ? Ag2 O4 2.380(2) . ? Ag2 O7 2.400(2) . ? Ag2 O8 2.425(2) . ? Ag2 O1 2.431(2) . ? Ag2 C28 2.462(3) . ? Ag2 C29 2.699(3) . ? Ag3 O7 2.348(2) . ? Ag3 O5 2.386(2) . ? Ag3 O4 2.436(2) . ? Ag3 C21 2.487(3) . ? Ag3 C22 2.565(4) . ? Ag3 O3 2.572(2) . ? Ag3 Ag4 3.3733(4) . ? Ag4 O2 2.364(2) . ? Ag4 O3 2.383(2) . ? Ag4 O6 2.420(2) . ? Ag4 C25 2.503(3) 6_556 ? Ag4 O5 2.531(2) . ? O1 C2 1.249(4) . ? O2 C4 1.259(4) . ? O3 C7 1.253(4) . ? O4 C9 1.261(4) . ? O5 C12 1.255(4) . ? O6 C14 1.263(4) . ? O7 C17 1.259(4) . ? O8 C19 1.251(4) . ? C1 F3 1.322(4) . ? C1 F2 1.334(4) . ? C1 F1 1.335(4) . ? C1 C2 1.545(4) . ? C2 C3 1.393(4) . ? C3 C4 1.392(4) . ? C4 C5 1.528(5) . ? C5 F5 1.331(4) . ? C5 F6 1.334(4) . ? C5 F4 1.335(4) . ? C6 F9 1.296(4) . ? C6 F7 1.319(4) . ? C6 F8 1.326(5) . ? C6 C7 1.536(5) . ? C7 C8 1.400(5) . ? C8 C9 1.395(4) . ? C9 C10 1.536(4) . ? C10 F11 1.319(4) . ? C10 F10 1.337(4) . ? C10 F12 1.340(4) . ? C11 F15 1.313(4) . ? C11 F14 1.319(4) . ? C11 F13 1.333(4) . ? C11 C12 1.537(5) . ? C12 C13 1.396(5) . ? C13 C14 1.395(4) . ? C14 C15 1.531(5) . ? C15 F17 1.326(4) . ? C15 F18 1.339(4) . ? C15 F16 1.339(4) . ? C16 F20 1.327(4) . ? C16 F21 1.328(4) . ? C16 F19 1.330(4) . ? C16 C17 1.533(4) . ? C17 C18 1.393(4) . ? C18 C19 1.399(4) . ? C19 C20 1.542(4) . ? C20 F22 1.323(4) . ? C20 F23 1.326(4) . ? C20 F24 1.330(4) . ? C21 C22 1.388(6) . ? C21 C26 1.395(6) . ? C22 C23 1.396(5) . ? C23 C24 1.386(5) . ? C24 C25 1.402(5) . ? C24 C27 1.509(5) . ? C25 C26 1.388(5) . ? C25 Ag4 2.503(3) 6 ? C28 C29 1.396(5) . ? C28 C33 1.398(5) . ? C29 C30 1.389(6) . ? C30 C31 1.378(6) . ? C30 Ag1 2.640(4) 6_565 ? C31 C32 1.391(6) . ? C31 Ag1 2.455(4) 6_565 ? C32 C33 1.388(5) . ? C33 C34 1.506(5) . ? 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 O2 Ag1 O6 77.57(7) . . ? O2 Ag1 O8 125.23(8) . . ? O6 Ag1 O8 89.60(8) . . ? O2 Ag1 C31 121.67(11) . 6_566 ? O6 Ag1 C31 117.17(13) . 6_566 ? O8 Ag1 C31 111.64(11) . 6_566 ? O2 Ag1 O1 73.53(7) . . ? O6 Ag1 O1 128.39(7) . . ? O8 Ag1 O1 74.21(7) . . ? C31 Ag1 O1 114.35(12) 6_566 . ? O2 Ag1 C30 110.51(11) . 6_566 ? O6 Ag1 C30 147.35(11) . 6_566 ? O8 Ag1 C30 108.36(10) . 6_566 ? C31 Ag1 C30 31.12(14) 6_566 6_566 ? O1 Ag1 C30 83.50(11) . 6_566 ? O4 Ag2 O7 79.88(7) . . ? O4 Ag2 O8 129.07(7) . . ? O7 Ag2 O8 73.82(7) . . ? O4 Ag2 O1 91.23(8) . . ? O7 Ag2 O1 130.43(8) . . ? O8 Ag2 O1 74.98(7) . . ? O4 Ag2 C28 122.83(10) . . ? O7 Ag2 C28 120.32(10) . . ? O8 Ag2 C28 108.09(10) . . ? O1 Ag2 C28 105.51(10) . . ? O4 Ag2 C29 101.76(10) . . ? O7 Ag2 C29 96.82(10) . . ? O8 Ag2 C29 123.81(10) . . ? O1 Ag2 C29 132.62(10) . . ? C28 Ag2 C29 30.94(11) . . ? O7 Ag3 O5 94.51(8) . . ? O7 Ag3 O4 79.77(7) . . ? O5 Ag3 O4 123.86(8) . . ? O7 Ag3 C21 136.63(11) . . ? O5 Ag3 C21 101.36(11) . . ? O4 Ag3 C21 120.84(11) . . ? O7 Ag3 C22 126.38(11) . . ? O5 Ag3 C22 131.77(11) . . ? O4 Ag3 C22 91.09(11) . . ? C21 Ag3 C22 31.84(13) . . ? O7 Ag3 O3 135.08(7) . . ? O5 Ag3 O3 76.02(7) . . ? O4 Ag3 O3 70.69(7) . . ? C21 Ag3 O3 88.11(10) . . ? C22 Ag3 O3 88.02(10) . . ? O7 Ag3 Ag4 96.39(6) . . ? O5 Ag3 Ag4 48.50(5) . . ? O4 Ag3 Ag4 76.42(5) . . ? C21 Ag3 Ag4 124.22(9) . . ? C22 Ag3 Ag4 132.78(9) . . ? O3 Ag3 Ag4 44.79(5) . . ? O2 Ag4 O3 101.09(8) . . ? O2 Ag4 O6 77.69(7) . . ? O3 Ag4 O6 131.73(8) . . ? O2 Ag4 C25 132.99(10) . 6_556 ? O3 Ag4 C25 112.67(10) . 6_556 ? O6 Ag4 C25 100.76(10) . 6_556 ? O2 Ag4 O5 135.34(8) . . ? O3 Ag4 O5 76.86(7) . . ? O6 Ag4 O5 72.17(7) . . ? C25 Ag4 O5 85.26(10) 6_556 . ? O2 Ag4 Ag3 99.82(6) . . ? O3 Ag4 Ag3 49.51(5) . . ? O6 Ag4 Ag3 82.74(6) . . ? C25 Ag4 Ag3 126.86(8) 6_556 . ? O5 Ag4 Ag3 44.91(5) . . ? C2 O1 Ag2 128.5(2) . . ? C2 O1 Ag1 121.32(19) . . ? Ag2 O1 Ag1 90.28(7) . . ? C4 O2 Ag4 133.4(2) . . ? C4 O2 Ag1 123.2(2) . . ? Ag4 O2 Ag1 103.42(8) . . ? C7 O3 Ag4 131.9(2) . . ? C7 O3 Ag3 119.26(19) . . ? Ag4 O3 Ag3 85.70(7) . . ? C9 O4 Ag2 135.5(2) . . ? C9 O4 Ag3 122.0(2) . . ? Ag2 O4 Ag3 99.14(7) . . ? C12 O5 Ag3 134.0(2) . . ? C12 O5 Ag4 120.8(2) . . ? Ag3 O5 Ag4 86.59(7) . . ? C14 O6 Ag1 134.9(2) . . ? C14 O6 Ag4 122.4(2) . . ? Ag1 O6 Ag4 101.30(7) . . ? C17 O7 Ag3 136.1(2) . . ? C17 O7 Ag2 122.9(2) . . ? Ag3 O7 Ag2 101.06(8) . . ? C19 O8 Ag1 128.9(2) . . ? C19 O8 Ag2 123.5(2) . . ? Ag1 O8 Ag2 91.68(7) . . ? F3 C1 F2 107.2(3) . . ? F3 C1 F1 107.5(3) . . ? F2 C1 F1 106.8(3) . . ? F3 C1 C2 112.3(3) . . ? F2 C1 C2 112.9(3) . . ? F1 C1 C2 109.9(3) . . ? O1 C2 C3 129.2(3) . . ? O1 C2 C1 114.3(3) . . ? C3 C2 C1 116.5(3) . . ? C4 C3 C2 123.6(3) . . ? O2 C4 C3 128.2(3) . . ? O2 C4 C5 114.0(3) . . ? C3 C4 C5 117.8(3) . . ? F5 C5 F6 106.6(3) . . ? F5 C5 F4 107.5(3) . . ? F6 C5 F4 106.4(3) . . ? F5 C5 C4 114.3(3) . . ? F6 C5 C4 110.6(3) . . ? F4 C5 C4 111.2(3) . . ? F9 C6 F7 108.2(3) . . ? F9 C6 F8 107.5(4) . . ? F7 C6 F8 104.6(3) . . ? F9 C6 C7 112.5(3) . . ? F7 C6 C7 114.5(3) . . ? F8 C6 C7 109.0(3) . . ? O3 C7 C8 128.8(3) . . ? O3 C7 C6 114.3(3) . . ? C8 C7 C6 116.7(3) . . ? C9 C8 C7 123.0(3) . . ? O4 C9 C8 128.3(3) . . ? O4 C9 C10 115.1(3) . . ? C8 C9 C10 116.4(3) . . ? F11 C10 F10 107.3(3) . . ? F11 C10 F12 107.3(3) . . ? F10 C10 F12 106.6(3) . . ? F11 C10 C9 114.5(3) . . ? F10 C10 C9 109.0(3) . . ? F12 C10 C9 111.8(3) . . ? F15 C11 F14 107.3(3) . . ? F15 C11 F13 106.9(3) . . ? F14 C11 F13 106.3(3) . . ? F15 C11 C12 112.5(3) . . ? F14 C11 C12 110.0(3) . . ? F13 C11 C12 113.4(3) . . ? O5 C12 C13 128.9(3) . . ? O5 C12 C11 114.1(3) . . ? C13 C12 C11 116.8(3) . . ? C14 C13 C12 123.5(3) . . ? O6 C14 C13 128.5(3) . . ? O6 C14 C15 114.8(3) . . ? C13 C14 C15 116.7(3) . . ? F17 C15 F18 107.3(3) . . ? F17 C15 F16 107.6(3) . . ? F18 C15 F16 106.5(3) . . ? F17 C15 C14 114.2(3) . . ? F18 C15 C14 111.5(3) . . ? F16 C15 C14 109.4(3) . . ? F20 C16 F21 106.6(3) . . ? F20 C16 F19 106.5(3) . . ? F21 C16 F19 106.8(3) . . ? F20 C16 C17 114.4(3) . . ? F21 C16 C17 111.4(3) . . ? F19 C16 C17 110.7(3) . . ? O7 C17 C18 128.2(3) . . ? O7 C17 C16 114.3(3) . . ? C18 C17 C16 117.5(3) . . ? C17 C18 C19 123.3(3) . . ? O8 C19 C18 128.6(3) . . ? O8 C19 C20 114.7(3) . . ? C18 C19 C20 116.7(3) . . ? F22 C20 F23 107.7(3) . . ? F22 C20 F24 106.6(3) . . ? F23 C20 F24 107.0(3) . . ? F22 C20 C19 110.4(3) . . ? F23 C20 C19 111.6(3) . . ? F24 C20 C19 113.3(3) . . ? C22 C21 C26 118.8(3) . . ? C22 C21 Ag3 77.2(2) . . ? C26 C21 Ag3 103.4(2) . . ? C21 C22 C23 121.0(4) . . ? C21 C22 Ag3 71.0(2) . . ? C23 C22 Ag3 106.9(2) . . ? C24 C23 C22 120.7(4) . . ? C23 C24 C25 117.8(3) . . ? C23 C24 C27 121.5(4) . . ? C25 C24 C27 120.7(4) . . ? C26 C25 C24 121.7(3) . . ? C26 C25 Ag4 87.7(2) . 6 ? C24 C25 Ag4 94.5(2) . 6 ? C25 C26 C21 119.8(4) . . ? C29 C28 C33 120.7(3) . . ? C29 C28 Ag2 84.0(2) . . ? C33 C28 Ag2 94.5(2) . . ? C30 C29 C28 120.0(4) . . ? C30 C29 Ag2 103.8(2) . . ? C28 C29 Ag2 65.09(18) . . ? C31 C30 C29 119.6(4) . . ? C31 C30 Ag1 67.0(2) . 6_565 ? C29 C30 Ag1 104.7(2) . 6_565 ? C30 C31 C32 120.3(4) . . ? C30 C31 Ag1 81.9(2) . 6_565 ? C32 C31 Ag1 97.9(2) . 6_565 ? C33 C32 C31 121.3(4) . . ? C32 C33 C28 118.1(4) . . ? C32 C33 C34 121.9(4) . . ? C28 C33 C34 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.011 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.097 #===END data_dg58 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Ag4 F24 O10' _chemical_formula_weight 1403.92 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' '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' _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 8.0252(3) _cell_length_b 11.2091(4) _cell_length_c 12.5306(5) _cell_angle_alpha 109.0870(10) _cell_angle_beta 106.2580(10) _cell_angle_gamma 94.9270(10) _cell_volume 1002.88(7) _cell_formula_units_Z 1 _cell_measurement_temperature 161(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 2.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5638 _exptl_absorpt_correction_T_max 0.8344 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 161(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 10703 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4713 _reflns_number_gt 4133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0454P)^2^+2.1746P] 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 SHELXTL _refine_ls_extinction_coef 0.0026(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4713 _refine_ls_number_parameters 295 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.77200(4) -0.18546(3) -0.26922(2) 0.03717(10) Uani 1 1 d . . . Ag2 Ag 0.79509(3) -0.01112(2) 0.03544(2) 0.02850(10) Uani 1 1 d . . . O1 O 0.9288(3) -0.1794(2) -0.0758(2) 0.0312(5) Uani 1 1 d . . . O2 O 1.0552(3) -0.0310(2) 0.1737(2) 0.0340(5) Uani 1 1 d . . . O3 O 0.5757(3) -0.0895(2) -0.1658(2) 0.0332(5) Uani 1 1 d . . . O4 O 0.6618(3) 0.1665(2) 0.0292(2) 0.0305(5) Uani 1 1 d . . . O5 O 0.7216(5) -0.3085(4) -0.4595(3) 0.0643(10) Uani 1 1 d . . . C1 C 0.9633(5) -0.3953(3) -0.1362(4) 0.0365(8) Uani 1 1 d . . . C2 C 0.9893(4) -0.2635(3) -0.0383(3) 0.0293(7) Uani 1 1 d . . . C3 C 1.0714(4) -0.2505(3) 0.0800(3) 0.0298(7) Uani 1 1 d . . . H3A H 1.1112 -0.3224 0.0957 0.036 Uiso 1 1 calc R . . C4 C 1.0968(4) -0.1367(3) 0.1753(3) 0.0306(7) Uani 1 1 d . . . C5 C 1.1833(6) -0.1351(4) 0.3016(4) 0.0428(9) Uani 1 1 d . . . C6 C 0.3091(5) -0.1294(5) -0.3239(4) 0.0449(9) Uani 1 1 d . . . C7 C 0.4451(5) -0.0424(4) -0.2017(3) 0.0322(7) Uani 1 1 d . . . C8 C 0.4060(5) 0.0771(4) -0.1479(3) 0.0315(7) Uani 1 1 d . . . H8A H 0.2952 0.0948 -0.1844 0.038 Uiso 1 1 calc R . . C9 C 0.5231(4) 0.1734(3) -0.0414(3) 0.0294(7) Uani 1 1 d . . . C10 C 0.4807(5) 0.3103(4) -0.0118(4) 0.0402(9) Uani 1 1 d . . . C11 C 0.7322(14) -0.4474(9) -0.5007(9) 0.061(2) Uiso 0.60 1 d P A 1 H11A H 0.8547 -0.4589 -0.4685 0.073 Uiso 0.60 1 calc PR A 1 H11B H 0.6530 -0.4963 -0.4748 0.073 Uiso 0.60 1 calc PR A 1 C12 C 0.6755(15) -0.4899(10) -0.6301(10) 0.075(3) Uiso 0.60 1 d P A 1 H12A H 0.5528 -0.5401 -0.6655 0.090 Uiso 0.60 1 calc PR A 1 H12B H 0.7539 -0.5448 -0.6619 0.090 Uiso 0.60 1 calc PR A 1 C13 C 0.6859(17) -0.3689(13) -0.6602(11) 0.080(3) Uiso 0.60 1 d P A 1 H13A H 0.5713 -0.3720 -0.7183 0.096 Uiso 0.60 1 calc PR A 1 H13B H 0.7782 -0.3664 -0.6982 0.096 Uiso 0.60 1 calc PR A 1 C14 C 0.7296(15) -0.2444(9) -0.5473(9) 0.059(2) Uiso 0.60 1 d P A 1 H14A H 0.8486 -0.1931 -0.5268 0.071 Uiso 0.60 1 calc PR A 1 H14B H 0.6396 -0.1900 -0.5554 0.071 Uiso 0.60 1 calc PR A 1 C11B C 0.802(2) -0.4107(16) -0.5033(14) 0.068(4) Uiso 0.40 1 d P A 2 H11C H 0.7291 -0.4942 -0.5192 0.081 Uiso 0.40 1 calc PR A 2 H11D H 0.9210 -0.4015 -0.4465 0.081 Uiso 0.40 1 calc PR A 2 C12B C 0.816(3) -0.399(2) -0.6211(18) 0.096(5) Uiso 0.40 1 d PD A 2 H12C H 0.9417 -0.3738 -0.6114 0.115 Uiso 0.40 1 calc PR A 2 H12D H 0.7692 -0.4847 -0.6863 0.115 Uiso 0.40 1 calc PR A 2 C13B C 0.721(4) -0.308(3) -0.655(3) 0.152(12) Uiso 0.40 1 d PD A 2 H13C H 0.6229 -0.3483 -0.7321 0.182 Uiso 0.40 1 calc PR A 2 H13D H 0.7987 -0.2359 -0.6569 0.182 Uiso 0.40 1 calc PR A 2 C14B C 0.658(3) -0.2711(18) -0.5522(16) 0.077(5) Uiso 0.40 1 d P A 2 H14C H 0.6793 -0.1759 -0.5194 0.092 Uiso 0.40 1 calc PR A 2 H14D H 0.5284 -0.3017 -0.5832 0.092 Uiso 0.40 1 calc PR A 2 F1 F 0.7970(4) -0.4571(3) -0.1743(3) 0.0812(11) Uani 1 1 d . . . F2 F 1.0642(4) -0.4725(2) -0.1022(2) 0.0520(6) Uani 1 1 d . . . F3 F 1.0007(5) -0.3826(3) -0.2295(2) 0.0610(8) Uani 1 1 d . . . F4 F 1.0723(5) -0.1102(4) 0.3638(3) 0.0833(11) Uani 1 1 d . . . F5 F 1.3263(4) -0.0423(3) 0.3614(3) 0.0681(8) Uani 1 1 d . . . F6 F 1.2317(5) -0.2438(3) 0.3052(3) 0.0735(10) Uani 1 1 d . . . F7 F 0.1831(5) -0.1962(5) -0.3103(3) 0.1101(17) Uani 1 1 d . . . F8 F 0.3790(5) -0.1999(4) -0.3945(3) 0.1068(16) Uani 1 1 d . . . F9 F 0.2202(7) -0.0630(4) -0.3822(3) 0.1192(19) Uani 1 1 d . . . F10 F 0.5248(5) 0.3724(3) 0.1035(3) 0.0849(12) Uani 1 1 d . . . F11 F 0.3122(3) 0.3119(2) -0.0604(3) 0.0544(7) Uani 1 1 d . . . F12 F 0.5719(4) 0.3779(3) -0.0537(4) 0.0710(10) 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 0.04369(18) 0.03666(17) 0.02603(15) 0.00605(11) 0.00824(12) 0.01439(12) Ag2 0.02819(14) 0.02868(14) 0.03074(15) 0.01345(11) 0.00789(10) 0.01199(10) O1 0.0334(12) 0.0304(12) 0.0325(12) 0.0150(10) 0.0089(10) 0.0124(10) O2 0.0341(13) 0.0316(12) 0.0350(13) 0.0140(11) 0.0055(10) 0.0123(10) O3 0.0332(13) 0.0386(13) 0.0308(12) 0.0146(11) 0.0107(10) 0.0143(10) O4 0.0275(11) 0.0316(12) 0.0381(13) 0.0176(10) 0.0122(10) 0.0109(9) O5 0.084(3) 0.067(2) 0.0345(16) 0.0072(15) 0.0149(16) 0.0371(19) C1 0.0380(19) 0.0303(17) 0.043(2) 0.0130(16) 0.0149(16) 0.0113(15) C2 0.0253(15) 0.0283(16) 0.0388(18) 0.0142(14) 0.0143(14) 0.0079(12) C3 0.0289(16) 0.0310(16) 0.0384(18) 0.0197(15) 0.0144(14) 0.0107(13) C4 0.0270(16) 0.0363(17) 0.0350(17) 0.0201(15) 0.0106(13) 0.0098(13) C5 0.051(2) 0.048(2) 0.037(2) 0.0241(18) 0.0137(18) 0.0185(19) C6 0.036(2) 0.059(3) 0.0332(19) 0.0111(18) 0.0076(16) 0.0102(18) C7 0.0318(17) 0.0413(19) 0.0286(16) 0.0179(15) 0.0114(14) 0.0081(14) C8 0.0289(16) 0.0417(19) 0.0348(18) 0.0244(15) 0.0124(14) 0.0138(14) C9 0.0290(16) 0.0321(16) 0.0388(18) 0.0198(14) 0.0187(14) 0.0127(13) C10 0.0329(18) 0.0347(19) 0.060(3) 0.0219(18) 0.0188(18) 0.0148(15) F1 0.0415(15) 0.0505(16) 0.108(3) -0.0207(17) 0.0214(16) -0.0045(12) F2 0.0718(17) 0.0352(12) 0.0562(15) 0.0195(11) 0.0237(13) 0.0269(12) F3 0.107(2) 0.0447(14) 0.0427(14) 0.0171(12) 0.0353(15) 0.0308(15) F4 0.089(2) 0.140(3) 0.0545(18) 0.057(2) 0.0410(17) 0.049(2) F5 0.0708(19) 0.0691(19) 0.0457(15) 0.0258(14) -0.0114(14) 0.0019(15) F6 0.111(3) 0.0602(17) 0.0499(16) 0.0340(14) 0.0041(16) 0.0388(17) F7 0.084(3) 0.139(4) 0.058(2) 0.004(2) 0.0100(19) -0.053(3) F8 0.059(2) 0.141(4) 0.0555(19) -0.036(2) 0.0037(15) 0.031(2) F9 0.146(4) 0.108(3) 0.052(2) 0.011(2) -0.033(2) 0.055(3) F10 0.116(3) 0.0604(19) 0.0620(19) 0.0050(15) 0.0144(19) 0.057(2) F11 0.0330(12) 0.0443(13) 0.094(2) 0.0332(14) 0.0200(13) 0.0198(10) F12 0.0526(16) 0.0478(15) 0.148(3) 0.0598(19) 0.0534(19) 0.0256(12) _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 O5 2.228(3) . ? Ag1 O1 2.373(2) . ? Ag1 O2 2.416(3) 2_755 ? Ag1 O3 2.416(2) . ? Ag2 O4 2.352(2) . ? Ag2 O2 2.391(2) . ? Ag2 O3 2.456(2) . ? Ag2 O1 2.474(2) . ? Ag2 C8 2.624(3) 2_655 ? O1 C2 1.258(4) . ? O2 C4 1.263(4) . ? O2 Ag1 2.416(3) 2_755 ? O3 C7 1.251(4) . ? O4 C9 1.239(4) . ? O5 C14B 1.345(18) . ? O5 C11B 1.396(16) . ? O5 C11 1.490(10) . ? O5 C14 1.510(11) . ? C1 F2 1.324(4) . ? C1 F1 1.325(5) . ? C1 F3 1.333(5) . ? C1 C2 1.533(5) . ? C2 C3 1.396(5) . ? C3 C4 1.385(5) . ? C4 C5 1.534(5) . ? C5 F6 1.321(5) . ? C5 F5 1.328(5) . ? C5 F4 1.329(5) . ? C6 F8 1.272(5) . ? C6 F7 1.289(6) . ? C6 F9 1.324(6) . ? C6 C7 1.547(5) . ? C7 C8 1.395(5) . ? C8 C9 1.418(5) . ? C8 Ag2 2.624(3) 2_655 ? C9 C10 1.547(5) . ? C10 F10 1.308(5) . ? C10 F11 1.323(4) . ? C10 F12 1.329(5) . ? C11 C12 1.453(14) . ? C12 C13 1.524(17) . ? C13 C14 1.555(16) . ? C11B C12B 1.55(2) . ? C12B C13B 1.43(2) . ? C13B C14B 1.46(4) . ? 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 O5 Ag1 O1 138.65(11) . . ? O5 Ag1 O2 124.13(13) . 2_755 ? O1 Ag1 O2 77.64(8) . 2_755 ? O5 Ag1 O3 131.48(12) . . ? O1 Ag1 O3 81.43(8) . . ? O2 Ag1 O3 82.59(9) 2_755 . ? O4 Ag2 O2 131.94(9) . . ? O4 Ag2 O3 76.21(8) . . ? O2 Ag2 O3 149.96(8) . . ? O4 Ag2 O1 143.64(8) . . ? O2 Ag2 O1 71.61(8) . . ? O3 Ag2 O1 78.66(8) . . ? O4 Ag2 C8 91.83(10) . 2_655 ? O2 Ag2 C8 91.65(10) . 2_655 ? O3 Ag2 C8 98.45(10) . 2_655 ? O1 Ag2 C8 117.68(10) . 2_655 ? C2 O1 Ag1 132.7(2) . . ? C2 O1 Ag2 123.5(2) . . ? Ag1 O1 Ag2 96.54(8) . . ? C4 O2 Ag2 124.6(2) . . ? C4 O2 Ag1 130.7(2) . 2_755 ? Ag2 O2 Ag1 103.61(9) . 2_755 ? C7 O3 Ag1 129.4(2) . . ? C7 O3 Ag2 127.3(2) . . ? Ag1 O3 Ag2 95.90(9) . . ? C9 O4 Ag2 130.7(2) . . ? C14B O5 C11B 104.5(11) . . ? C14B O5 C11 111.5(9) . . ? C11B O5 C11 27.2(7) . . ? C14B O5 C14 23.3(8) . . ? C11B O5 C14 97.7(8) . . ? C11 O5 C14 114.9(6) . . ? C14B O5 Ag1 124.2(8) . . ? C11B O5 Ag1 127.5(7) . . ? C11 O5 Ag1 123.9(4) . . ? C14 O5 Ag1 118.8(4) . . ? F2 C1 F1 106.9(3) . . ? F2 C1 F3 106.0(3) . . ? F1 C1 F3 107.9(4) . . ? F2 C1 C2 114.4(3) . . ? F1 C1 C2 110.5(3) . . ? F3 C1 C2 110.9(3) . . ? O1 C2 C3 127.6(3) . . ? O1 C2 C1 114.6(3) . . ? C3 C2 C1 117.7(3) . . ? C4 C3 C2 122.4(3) . . ? O2 C4 C3 128.7(3) . . ? O2 C4 C5 113.5(3) . . ? C3 C4 C5 117.7(3) . . ? F6 C5 F5 107.0(4) . . ? F6 C5 F4 107.3(4) . . ? F5 C5 F4 106.3(4) . . ? F6 C5 C4 114.5(3) . . ? F5 C5 C4 111.3(3) . . ? F4 C5 C4 110.1(3) . . ? F8 C6 F7 111.8(5) . . ? F8 C6 F9 105.9(4) . . ? F7 C6 F9 101.3(5) . . ? F8 C6 C7 113.3(3) . . ? F7 C6 C7 111.1(4) . . ? F9 C6 C7 112.7(4) . . ? O3 C7 C8 129.3(3) . . ? O3 C7 C6 114.8(3) . . ? C8 C7 C6 115.8(3) . . ? C7 C8 C9 123.4(3) . . ? C7 C8 Ag2 99.6(2) . 2_655 ? C9 C8 Ag2 92.6(2) . 2_655 ? O4 C9 C8 129.5(3) . . ? O4 C9 C10 114.2(3) . . ? C8 C9 C10 116.2(3) . . ? F10 C10 F11 107.7(4) . . ? F10 C10 F12 107.4(4) . . ? F11 C10 F12 106.1(3) . . ? F10 C10 C9 111.7(3) . . ? F11 C10 C9 113.8(3) . . ? F12 C10 C9 109.6(3) . . ? C12 C11 O5 104.7(8) . . ? C11 C12 C13 106.7(9) . . ? C12 C13 C14 112.0(10) . . ? O5 C14 C13 97.5(8) . . ? O5 C11B C12B 103.0(13) . . ? C13B C12B C11B 114(2) . . ? C12B C13B C14B 95(2) . . ? O5 C14B C13B 121.7(17) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.649 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.109 #===END data_dg60 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 Ag3 F18 O6 Si' _chemical_formula_weight 1045.02 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' '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3415(5) _cell_length_b 11.7534(5) _cell_length_c 13.3836(5) _cell_angle_alpha 93.6360(10) _cell_angle_beta 103.6640(10) _cell_angle_gamma 114.4510(10) _cell_volume 1551.66(11) _cell_formula_units_Z 2 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 2.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5775 _exptl_absorpt_correction_T_max 0.6605 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 165(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 16519 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7252 _reflns_number_gt 6654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0376P)^2^+5.2974P] 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 7252 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.009 _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 0.27760(3) 0.61291(2) 0.19984(2) 0.02574(7) Uani 1 1 d . . . Ag2 Ag -0.05684(3) 0.44583(3) 0.09729(2) 0.02590(7) Uani 1 1 d . . . Ag3 Ag 0.02778(3) 0.47342(3) 0.36959(2) 0.02958(8) Uani 1 1 d . . . Si1 Si 0.60282(12) 0.86127(13) 0.30711(11) 0.0440(3) Uani 1 1 d . . . O1 O 0.1417(2) 0.4521(2) 0.03170(19) 0.0249(5) Uani 1 1 d . . . O2 O 0.1056(3) 0.3951(2) 0.2252(2) 0.0272(5) Uani 1 1 d . A . O3 O 0.1700(3) 0.7063(2) 0.0754(2) 0.0292(5) Uani 1 1 d . . . O4 O 0.1189(3) 0.6480(2) 0.2675(2) 0.0292(5) Uani 1 1 d . A . O5 O -0.1720(3) 0.3781(3) 0.2265(2) 0.0333(6) Uani 1 1 d . A . O6 O -0.1486(3) 0.4567(3) 0.4502(2) 0.0361(6) Uani 1 1 d . . . C1 C 0.4762(5) 0.5970(5) 0.2105(5) 0.0564(14) Uani 1 1 d . A . C2 C 0.5093(7) 0.6820(6) 0.2873(5) 0.0387(14) Uiso 0.65 1 d P A 1 C3 C 0.5184(11) 0.9305(11) 0.3707(9) 0.067(3) Uiso 0.65 1 d P A 1 H3A H 0.5238 0.9097 0.4409 0.100 Uiso 0.65 1 calc PR A 1 H3B H 0.4233 0.8965 0.3297 0.100 Uiso 0.65 1 calc PR A 1 H3C H 0.5622 1.0231 0.3761 0.100 Uiso 0.65 1 calc PR A 1 C4 C 0.5942(10) 0.9012(9) 0.1684(7) 0.062(2) Uiso 0.65 1 d P A 1 H4A H 0.6404 0.8629 0.1348 0.092 Uiso 0.65 1 calc PR A 1 H4B H 0.6384 0.9937 0.1734 0.092 Uiso 0.65 1 calc PR A 1 H4C H 0.4993 0.8673 0.1268 0.092 Uiso 0.65 1 calc PR A 1 C5 C 0.7801(9) 0.9066(9) 0.3746(7) 0.062(2) Uiso 0.65 1 d P A 1 H5A H 0.8076 0.8458 0.3461 0.094 Uiso 0.65 1 calc PR A 1 H5B H 0.7913 0.9063 0.4495 0.094 Uiso 0.65 1 calc PR A 1 H5C H 0.8364 0.9919 0.3645 0.094 Uiso 0.65 1 calc PR A 1 C2B C 0.5083(12) 0.7123(11) 0.2135(9) 0.034(2) Uiso 0.35 1 d P A 2 C3B C 0.5047(19) 0.9515(17) 0.3389(15) 0.057(4) Uiso 0.35 1 d P A 2 H3BA H 0.4541 0.9641 0.2738 0.085 Uiso 0.35 1 calc PR A 2 H3BB H 0.5683 1.0343 0.3830 0.085 Uiso 0.35 1 calc PR A 2 H3BC H 0.4415 0.9022 0.3762 0.085 Uiso 0.35 1 calc PR A 2 C4B C 0.734(2) 0.984(2) 0.2643(18) 0.088(6) Uiso 0.35 1 d P A 2 H4BA H 0.7939 0.9502 0.2461 0.132 Uiso 0.35 1 calc PR A 2 H4BB H 0.7876 1.0580 0.3209 0.132 Uiso 0.35 1 calc PR A 2 H4BC H 0.6920 1.0096 0.2029 0.132 Uiso 0.35 1 calc PR A 2 C5B C 0.698(2) 0.830(2) 0.4321(17) 0.086(6) Uiso 0.35 1 d P A 2 H5BA H 0.7467 0.7832 0.4144 0.130 Uiso 0.35 1 calc PR A 2 H5BB H 0.6332 0.7792 0.4679 0.130 Uiso 0.35 1 calc PR A 2 H5BC H 0.7624 0.9110 0.4783 0.130 Uiso 0.35 1 calc PR A 2 C6 C 0.2202(4) 0.3310(4) -0.0593(3) 0.0317(8) Uani 1 1 d . A . F1 F 0.1874(3) 0.2086(2) -0.0865(2) 0.0495(7) Uani 1 1 d . . . F2 F 0.3562(2) 0.3944(3) -0.0308(2) 0.0451(6) Uani 1 1 d . . . F3 F 0.1754(2) 0.3711(2) -0.14456(17) 0.0371(5) Uani 1 1 d . . . C7 C 0.1680(3) 0.3577(3) 0.0311(3) 0.0251(7) Uani 1 1 d . . . C8 C 0.1625(4) 0.2813(3) 0.1064(3) 0.0286(7) Uani 1 1 d . A . H8A H 0.1828 0.2114 0.0964 0.034 Uiso 1 1 calc R . . C9 C 0.1277(4) 0.3046(3) 0.1967(3) 0.0270(7) Uani 1 1 d . . . C10 C 0.1181(5) 0.2072(4) 0.2704(3) 0.0385(9) Uani 1 1 d . A . C11 C 0.1919(4) 0.9056(4) 0.0365(3) 0.0352(8) Uani 1 1 d . A . C12 C 0.1630(4) 0.8046(3) 0.1069(3) 0.0272(7) Uani 1 1 d . . . C13 C 0.1379(4) 0.8354(3) 0.1998(3) 0.0322(8) Uani 1 1 d . A . H13A H 0.1346 0.9141 0.2140 0.039 Uiso 1 1 calc R . . C14 C 0.1176(4) 0.7548(3) 0.2721(3) 0.0304(7) Uani 1 1 d . . . C15 C 0.0902(5) 0.7984(4) 0.3711(4) 0.0445(10) Uani 1 1 d . A . C16 C -0.3941(4) 0.2816(4) 0.1145(3) 0.0302(7) Uani 1 1 d . A . C17 C -0.2923(4) 0.3477(3) 0.2230(3) 0.0271(7) Uani 1 1 d . . . C18 C -0.3469(4) 0.3622(4) 0.3028(3) 0.0350(9) Uani 1 1 d . A . H18A H -0.4420 0.3335 0.2852 0.042 Uiso 1 1 calc R . . C19 C -0.2720(4) 0.4158(5) 0.4065(3) 0.0381(9) Uani 1 1 d . . . F4 F 0.2396(4) 0.2151(4) 0.3150(3) 0.0791(11) Uani 1 1 d . . . F5 F 0.0656(4) 0.2237(3) 0.3442(3) 0.0706(10) Uani 1 1 d . . . F6 F 0.0433(3) 0.0883(2) 0.2188(2) 0.0571(8) Uani 1 1 d . . . F7 F 0.3229(3) 0.9865(3) 0.0671(3) 0.0627(9) Uani 1 1 d . . . F8 F 0.1220(3) 0.9734(2) 0.0394(2) 0.0515(7) Uani 1 1 d . . . F9 F 0.1623(3) 0.8546(2) -0.06289(19) 0.0394(5) Uani 1 1 d . . . F10 F 0.1861(4) 0.8095(4) 0.4555(2) 0.0796(11) Uani 1 1 d . . . F11 F 0.0831(5) 0.9076(3) 0.3738(3) 0.0782(12) Uani 1 1 d . . . F12 F -0.0244(4) 0.7125(3) 0.3821(3) 0.0697(10) Uani 1 1 d . . . F13 F -0.4029(3) 0.1680(3) 0.0876(2) 0.0517(7) Uani 1 1 d . . . F14 F -0.5193(2) 0.2663(3) 0.10784(19) 0.0438(6) Uani 1 1 d . . . F15 F -0.3548(3) 0.3492(3) 0.04147(18) 0.0510(7) Uani 1 1 d . . . C20 C -0.3609(8) 0.4027(8) 0.4806(6) 0.0314(15) Uiso 0.50 1 d P A 1 F16 F -0.3500(10) 0.3397(9) 0.5495(7) 0.094(3) Uiso 0.50 1 d P A 1 F17 F -0.2989(8) 0.5211(8) 0.5515(6) 0.0740(19) Uiso 0.50 1 d P A 1 F18 F -0.4854(6) 0.3714(6) 0.4414(4) 0.0462(12) Uiso 0.50 1 d P A 1 C20B C -0.3447(11) 0.4627(11) 0.4747(8) 0.047(2) Uiso 0.50 1 d P A 2 F16B F -0.3034(12) 0.5883(11) 0.4883(9) 0.116(3) Uiso 0.50 1 d P A 2 F17B F -0.3069(6) 0.4554(6) 0.5699(5) 0.0535(14) Uiso 0.50 1 d P A 2 F18B F -0.4701(5) 0.4298(5) 0.4327(4) 0.0400(11) Uiso 0.50 1 d P A 2 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 0.02037(12) 0.02472(13) 0.03050(14) 0.00183(10) 0.00583(10) 0.00970(10) Ag2 0.02640(13) 0.03425(14) 0.02209(12) 0.00789(10) 0.00931(10) 0.01655(11) Ag3 0.02249(13) 0.04569(17) 0.02113(13) 0.00601(11) 0.00775(10) 0.01486(12) Si1 0.0243(5) 0.0447(7) 0.0521(7) -0.0018(5) 0.0060(5) 0.0090(5) O1 0.0269(12) 0.0215(11) 0.0282(12) 0.0049(9) 0.0093(10) 0.0118(10) O2 0.0296(13) 0.0259(12) 0.0295(12) 0.0062(10) 0.0104(10) 0.0145(10) O3 0.0348(14) 0.0250(12) 0.0294(13) 0.0035(10) 0.0077(11) 0.0160(11) O4 0.0311(13) 0.0268(12) 0.0339(13) 0.0067(10) 0.0143(11) 0.0142(11) O5 0.0227(12) 0.0491(16) 0.0253(12) 0.0061(11) 0.0081(10) 0.0128(12) O6 0.0248(13) 0.0611(18) 0.0243(12) 0.0088(12) 0.0080(10) 0.0202(13) C1 0.025(2) 0.052(3) 0.090(4) -0.004(3) 0.011(2) 0.020(2) C6 0.0328(19) 0.0331(18) 0.0334(19) 0.0044(15) 0.0132(15) 0.0169(16) F1 0.0759(19) 0.0378(13) 0.0499(15) 0.0043(11) 0.0314(14) 0.0328(14) F2 0.0320(12) 0.0669(17) 0.0438(14) 0.0101(12) 0.0174(11) 0.0255(12) F3 0.0409(13) 0.0440(13) 0.0289(11) 0.0059(10) 0.0122(10) 0.0201(11) C7 0.0223(16) 0.0217(15) 0.0295(17) 0.0012(13) 0.0079(13) 0.0084(13) C8 0.0326(18) 0.0230(16) 0.0363(19) 0.0061(14) 0.0127(15) 0.0163(14) C9 0.0276(17) 0.0238(16) 0.0296(17) 0.0080(13) 0.0073(14) 0.0114(14) C10 0.051(2) 0.037(2) 0.038(2) 0.0147(17) 0.0180(19) 0.0256(19) C11 0.034(2) 0.0239(17) 0.044(2) 0.0078(16) 0.0121(17) 0.0090(15) C12 0.0228(16) 0.0221(15) 0.0341(18) 0.0045(13) 0.0068(14) 0.0083(13) C13 0.038(2) 0.0212(16) 0.039(2) 0.0016(14) 0.0138(16) 0.0143(15) C14 0.0323(19) 0.0262(17) 0.0357(19) 0.0029(14) 0.0128(15) 0.0144(15) C15 0.062(3) 0.038(2) 0.043(2) 0.0052(18) 0.023(2) 0.028(2) C16 0.0248(17) 0.0342(19) 0.0289(17) 0.0068(14) 0.0103(14) 0.0090(15) C17 0.0249(17) 0.0319(18) 0.0244(16) 0.0088(14) 0.0069(13) 0.0120(14) C18 0.0214(17) 0.059(3) 0.0256(17) 0.0101(17) 0.0083(14) 0.0179(17) C19 0.0276(19) 0.066(3) 0.0261(18) 0.0109(18) 0.0105(15) 0.0238(19) F4 0.066(2) 0.101(3) 0.081(2) 0.056(2) 0.0111(18) 0.047(2) F5 0.130(3) 0.0603(19) 0.0623(19) 0.0374(16) 0.063(2) 0.057(2) F6 0.084(2) 0.0308(13) 0.0605(18) 0.0208(12) 0.0263(16) 0.0248(14) F7 0.0398(15) 0.0469(16) 0.0681(19) 0.0194(14) 0.0076(14) -0.0092(12) F8 0.081(2) 0.0376(13) 0.0569(16) 0.0192(12) 0.0269(15) 0.0405(14) F9 0.0456(14) 0.0398(13) 0.0396(13) 0.0153(10) 0.0179(11) 0.0213(11) F10 0.097(3) 0.111(3) 0.0366(16) -0.0081(17) 0.0090(17) 0.059(2) F11 0.150(4) 0.0564(19) 0.072(2) 0.0180(16) 0.066(2) 0.067(2) F12 0.084(2) 0.066(2) 0.076(2) 0.0114(17) 0.058(2) 0.0304(18) F13 0.0419(14) 0.0405(14) 0.0597(17) -0.0090(12) 0.0015(12) 0.0155(12) F14 0.0253(11) 0.0630(16) 0.0365(13) 0.0016(11) 0.0014(9) 0.0185(11) F15 0.0402(14) 0.0608(17) 0.0250(11) 0.0127(11) 0.0026(10) -0.0002(12) _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 C1 2.308(4) . ? Ag1 C2B 2.337(12) . ? Ag1 O4 2.359(3) . ? Ag1 C2 2.365(7) . ? Ag1 O3 2.418(3) . ? Ag1 O1 2.534(2) . ? Ag1 Ag2 3.3406(4) . ? Ag2 O5 2.390(3) . ? Ag2 O1 2.404(2) 2_565 ? Ag2 O2 2.496(3) . ? Ag2 O3 2.522(3) 2_565 ? Ag2 O1 2.579(2) . ? Ag2 Ag2 3.2731(5) 2_565 ? Ag3 O6 2.372(3) 2_566 ? Ag3 O5 2.373(3) . ? Ag3 O6 2.434(3) . ? Ag3 O4 2.533(3) . ? Ag3 O2 2.571(2) . ? Si1 C3 1.802(11) . ? Si1 C2B 1.821(11) . ? Si1 C5 1.826(9) . ? Si1 C4B 1.83(2) . ? Si1 C2 1.892(7) . ? Si1 C5B 1.91(2) . ? Si1 C3B 1.921(18) . ? Si1 C4 1.933(9) . ? O1 C7 1.262(4) . ? O1 Ag2 2.404(2) 2_565 ? O2 C9 1.247(4) . ? O3 C12 1.244(4) . ? O3 Ag2 2.522(3) 2_565 ? O4 C14 1.258(4) . ? O5 C17 1.247(4) . ? O6 C19 1.246(5) . ? O6 Ag3 2.372(3) 2_566 ? C1 C2B 1.245(12) . ? C1 C2 1.254(8) . ? C6 F1 1.329(4) . ? C6 F3 1.332(5) . ? C6 F2 1.347(5) . ? C6 C7 1.535(5) . ? C7 C8 1.387(5) . ? C8 C9 1.403(5) . ? C9 C10 1.544(5) . ? C10 F5 1.311(5) . ? C10 F4 1.328(6) . ? C10 F6 1.330(5) . ? C11 F9 1.327(5) . ? C11 F7 1.331(5) . ? C11 F8 1.341(5) . ? C11 C12 1.540(5) . ? C12 C13 1.399(5) . ? C13 C14 1.388(5) . ? C14 C15 1.535(6) . ? C15 F11 1.317(5) . ? C15 F12 1.325(6) . ? C15 F10 1.328(6) . ? C16 F13 1.317(5) . ? C16 F14 1.336(4) . ? C16 F15 1.340(4) . ? C16 C17 1.538(5) . ? C17 C18 1.389(5) . ? C18 C19 1.391(5) . ? C19 C20 1.546(9) . ? C19 C20B 1.576(11) . ? C20 F16 1.233(12) . ? C20 F18 1.265(10) . ? C20 F17 1.428(11) . ? C20B F17B 1.266(12) . ? C20B F18B 1.276(11) . ? C20B F16B 1.335(15) . ? 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 C1 Ag1 C2B 31.1(3) . . ? C1 Ag1 O4 155.12(17) . . ? C2B Ag1 O4 139.5(3) . . ? C1 Ag1 C2 31.1(2) . . ? C2B Ag1 C2 26.3(3) . . ? O4 Ag1 C2 126.52(17) . . ? C1 Ag1 O3 127.67(18) . . ? C2B Ag1 O3 106.7(3) . . ? O4 Ag1 O3 72.64(9) . . ? C2 Ag1 O3 129.96(18) . . ? C1 Ag1 O1 95.45(15) . . ? C2B Ag1 O1 111.9(3) . . ? O4 Ag1 O1 105.99(9) . . ? C2 Ag1 O1 126.50(17) . . ? O3 Ag1 O1 70.94(8) . . ? C1 Ag1 Ag2 140.78(13) . . ? C2B Ag1 Ag2 160.8(3) . . ? O4 Ag1 Ag2 56.62(6) . . ? C2 Ag1 Ag2 165.23(16) . . ? O3 Ag1 Ag2 64.39(6) . . ? O1 Ag1 Ag2 49.79(5) . . ? O5 Ag2 O1 118.15(9) . 2_565 ? O5 Ag2 O2 77.98(9) . . ? O1 Ag2 O2 160.37(8) 2_565 . ? O5 Ag2 O3 113.44(9) . 2_565 ? O1 Ag2 O3 71.36(8) 2_565 2_565 ? O2 Ag2 O3 114.18(8) . 2_565 ? O5 Ag2 O1 143.88(9) . . ? O1 Ag2 O1 97.96(7) 2_565 . ? O2 Ag2 O1 66.85(8) . . ? O3 Ag2 O1 75.87(8) 2_565 . ? O5 Ag2 Ag2 169.42(7) . 2_565 ? O1 Ag2 Ag2 51.29(6) 2_565 2_565 ? O2 Ag2 Ag2 112.46(6) . 2_565 ? O3 Ag2 Ag2 64.72(6) 2_565 2_565 ? O1 Ag2 Ag2 46.67(5) . 2_565 ? O5 Ag2 Ag1 112.88(6) . . ? O1 Ag2 Ag1 110.37(6) 2_565 . ? O2 Ag2 Ag1 50.42(6) . . ? O3 Ag2 Ag1 124.48(6) 2_565 . ? O1 Ag2 Ag1 48.63(5) . . ? Ag2 Ag2 Ag1 74.628(11) 2_565 . ? O6 Ag3 O5 153.92(9) 2_566 . ? O6 Ag3 O6 77.44(10) 2_566 . ? O5 Ag3 O6 76.99(9) . . ? O6 Ag3 O4 110.45(10) 2_566 . ? O5 Ag3 O4 87.44(9) . . ? O6 Ag3 O4 121.59(9) . . ? O6 Ag3 O2 126.43(9) 2_566 . ? O5 Ag3 O2 76.80(9) . . ? O6 Ag3 O2 150.69(9) . . ? O4 Ag3 O2 69.92(8) . . ? C3 Si1 C2B 121.3(5) . . ? C3 Si1 C5 116.4(5) . . ? C2B Si1 C5 118.0(5) . . ? C3 Si1 C4B 110.4(8) . . ? C2B Si1 C4B 113.6(8) . . ? C5 Si1 C4B 61.3(8) . . ? C3 Si1 C2 109.2(4) . . ? C2B Si1 C2 33.4(4) . . ? C5 Si1 C2 107.3(4) . . ? C4B Si1 C2 139.5(8) . . ? C3 Si1 C5B 95.4(8) . . ? C2B Si1 C5B 108.2(8) . . ? C5 Si1 C5B 44.5(7) . . ? C4B Si1 C5B 105.0(10) . . ? C2 Si1 C5B 79.3(7) . . ? C3 Si1 C3B 15.9(6) . . ? C2B Si1 C3B 117.6(7) . . ? C5 Si1 C3B 124.1(6) . . ? C4B Si1 C3B 100.9(9) . . ? C2 Si1 C3B 115.4(6) . . ? C5B Si1 C3B 110.6(9) . . ? C3 Si1 C4 110.4(5) . . ? C2B Si1 C4 72.2(5) . . ? C5 Si1 C4 107.4(4) . . ? C4B Si1 C4 51.8(8) . . ? C2 Si1 C4 105.6(3) . . ? C5B Si1 C4 149.7(8) . . ? C3B Si1 C4 94.5(7) . . ? C7 O1 Ag2 136.3(2) . 2_565 ? C7 O1 Ag1 111.6(2) . . ? Ag2 O1 Ag1 108.54(9) 2_565 . ? C7 O1 Ag2 120.0(2) . . ? Ag2 O1 Ag2 82.04(7) 2_565 . ? Ag1 O1 Ag2 81.58(7) . . ? C9 O2 Ag2 118.4(2) . . ? C9 O2 Ag3 140.2(2) . . ? Ag2 O2 Ag3 87.36(8) . . ? C12 O3 Ag1 119.2(2) . . ? C12 O3 Ag2 131.5(2) . 2_565 ? Ag1 O3 Ag2 108.50(9) . 2_565 ? C14 O4 Ag1 120.2(2) . . ? C14 O4 Ag3 129.6(2) . . ? Ag1 O4 Ag3 107.35(10) . . ? C17 O5 Ag3 130.6(2) . . ? C17 O5 Ag2 130.1(2) . . ? Ag3 O5 Ag2 94.57(9) . . ? C19 O6 Ag3 129.6(2) . 2_566 ? C19 O6 Ag3 127.7(2) . . ? Ag3 O6 Ag3 102.56(10) 2_566 . ? C2B C1 C2 50.7(6) . . ? C2B C1 Ag1 75.7(6) . . ? C2 C1 Ag1 76.9(4) . . ? C1 C2 Si1 131.6(6) . . ? C1 C2 Ag1 72.0(4) . . ? Si1 C2 Ag1 110.0(3) . . ? C1 C2B Si1 139.3(9) . . ? C1 C2B Ag1 73.2(6) . . ? Si1 C2B Ag1 114.0(5) . . ? F1 C6 F3 107.8(3) . . ? F1 C6 F2 107.3(3) . . ? F3 C6 F2 106.4(3) . . ? F1 C6 C7 113.2(3) . . ? F3 C6 C7 112.4(3) . . ? F2 C6 C7 109.4(3) . . ? O1 C7 C8 126.9(3) . . ? O1 C7 C6 115.9(3) . . ? C8 C7 C6 117.1(3) . . ? C7 C8 C9 121.6(3) . . ? O2 C9 C8 127.9(3) . . ? O2 C9 C10 116.4(3) . . ? C8 C9 C10 115.7(3) . . ? F5 C10 F4 108.4(4) . . ? F5 C10 F6 107.6(4) . . ? F4 C10 F6 105.8(4) . . ? F5 C10 C9 112.3(3) . . ? F4 C10 C9 110.6(4) . . ? F6 C10 C9 111.9(3) . . ? F9 C11 F7 107.1(3) . . ? F9 C11 F8 107.2(3) . . ? F7 C11 F8 107.7(3) . . ? F9 C11 C12 112.1(3) . . ? F7 C11 C12 109.8(3) . . ? F8 C11 C12 112.7(3) . . ? O3 C12 C13 127.7(3) . . ? O3 C12 C11 115.3(3) . . ? C13 C12 C11 116.9(3) . . ? C14 C13 C12 122.1(3) . . ? O4 C14 C13 128.1(3) . . ? O4 C14 C15 114.4(3) . . ? C13 C14 C15 117.5(3) . . ? F11 C15 F12 107.5(4) . . ? F11 C15 F10 107.7(4) . . ? F12 C15 F10 105.6(4) . . ? F11 C15 C14 114.4(4) . . ? F12 C15 C14 110.9(4) . . ? F10 C15 C14 110.3(4) . . ? F13 C16 F14 106.9(3) . . ? F13 C16 F15 107.2(3) . . ? F14 C16 F15 106.6(3) . . ? F13 C16 C17 111.2(3) . . ? F14 C16 C17 113.9(3) . . ? F15 C16 C17 110.5(3) . . ? O5 C17 C18 129.4(3) . . ? O5 C17 C16 114.5(3) . . ? C18 C17 C16 116.1(3) . . ? C17 C18 C19 124.6(3) . . ? O6 C19 C18 130.6(4) . . ? O6 C19 C20 115.5(4) . . ? C18 C19 C20 113.2(4) . . ? O6 C19 C20B 112.3(5) . . ? C18 C19 C20B 115.3(5) . . ? C20 C19 C20B 24.7(4) . . ? F16 C20 F18 108.0(8) . . ? F16 C20 F17 94.6(8) . . ? F18 C20 F17 109.8(7) . . ? F16 C20 C19 116.4(8) . . ? F18 C20 C19 118.7(6) . . ? F17 C20 C19 106.5(6) . . ? F17B C20B F18B 118.1(9) . . ? F17B C20B F16B 97.3(9) . . ? F18B C20B F16B 97.3(9) . . ? F17B C20B C19 112.1(8) . . ? F18B C20B C19 115.9(8) . . ? F16B C20B C19 113.3(9) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 2.074 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.111 #===END data_dg61 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Ag F6 O2 Si2' _chemical_formula_weight 485.33 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' '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1679(10) _cell_length_b 9.4922(7) _cell_length_c 16.3439(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.8260(10) _cell_angle_gamma 90.00 _cell_volume 2006.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.8618 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 165(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 18471 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4110 _reflns_number_gt 3176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0609P)^2^+2.1883P] 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 4110 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.12577(2) 0.08519(3) 0.146004(19) 0.03313(13) Uani 1 1 d . . . Si1 Si 0.35896(9) -0.08147(12) 0.15136(7) 0.0331(3) Uani 1 1 d . . . Si2 Si 0.15572(8) 0.27533(11) -0.02864(7) 0.0291(2) Uani 1 1 d . . . O1 O 0.0872(2) -0.0231(3) 0.25844(17) 0.0340(6) Uani 1 1 d . . . O2 O -0.0347(2) 0.1742(3) 0.13510(18) 0.0383(7) Uani 1 1 d . . . C1 C 0.2730(3) 0.0589(4) 0.0946(3) 0.0333(9) Uani 1 1 d . . . C2 C 0.2212(3) 0.1470(4) 0.0508(2) 0.0315(8) Uani 1 1 d . . . C3 C 0.4190(4) -0.0106(6) 0.2548(3) 0.0563(13) Uani 1 1 d . . . H3A H 0.3650 0.0112 0.2867 0.085 Uiso 1 1 calc R . . H3B H 0.4575 0.0755 0.2474 0.085 Uiso 1 1 calc R . . H3C H 0.4664 -0.0808 0.2849 0.085 Uiso 1 1 calc R . . C4 C 0.4574(4) -0.1254(6) 0.0886(3) 0.0541(13) Uani 1 1 d . . . H4A H 0.5015 -0.0432 0.0855 0.081 Uiso 1 1 calc R . . H4B H 0.4231 -0.1524 0.0322 0.081 Uiso 1 1 calc R . . H4C H 0.4998 -0.2041 0.1146 0.081 Uiso 1 1 calc R . . C5 C 0.2718(4) -0.2319(5) 0.1605(3) 0.0487(12) Uani 1 1 d . . . H5A H 0.2210 -0.2038 0.1942 0.073 Uiso 1 1 calc R . . H5B H 0.3125 -0.3114 0.1872 0.073 Uiso 1 1 calc R . . H5C H 0.2357 -0.2599 0.1048 0.073 Uiso 1 1 calc R . . C6 C 0.1460(4) 0.4470(5) 0.0227(4) 0.0512(13) Uani 1 1 d . . . H6A H 0.1030 0.4368 0.0651 0.077 Uiso 1 1 calc R . . H6B H 0.1148 0.5163 -0.0190 0.077 Uiso 1 1 calc R . . H6C H 0.2153 0.4787 0.0490 0.077 Uiso 1 1 calc R . . C7 C 0.2360(4) 0.2859(5) -0.1098(3) 0.0490(12) Uani 1 1 d . . . H7A H 0.2393 0.1929 -0.1353 0.074 Uiso 1 1 calc R . . H7B H 0.3059 0.3166 -0.0846 0.074 Uiso 1 1 calc R . . H7C H 0.2053 0.3537 -0.1526 0.074 Uiso 1 1 calc R . . C8 C 0.0251(3) 0.2024(5) -0.0700(3) 0.0420(10) Uani 1 1 d . . . H8A H 0.0320 0.1115 -0.0969 0.063 Uiso 1 1 calc R . . H8B H -0.0132 0.2680 -0.1108 0.063 Uiso 1 1 calc R . . H8C H -0.0124 0.1892 -0.0241 0.063 Uiso 1 1 calc R . . C9 C 0.0046(3) -0.0975(5) 0.3652(3) 0.0382(10) Uani 1 1 d . . . C10 C 0.0039(3) -0.0161(4) 0.2839(2) 0.0306(8) Uani 1 1 d . . . C11 C -0.0877(3) 0.0529(4) 0.2491(2) 0.0325(9) Uani 1 1 d . . . H11 H -0.1460 0.0406 0.2750 0.039 Uiso 1 1 calc R . . C12 C -0.0990(3) 0.1394(4) 0.1784(2) 0.0310(8) Uani 1 1 d . . . C13 C -0.2048(3) 0.2119(5) 0.1513(3) 0.0425(10) Uani 1 1 d . . . F1 F 0.0846(2) -0.0625(4) 0.42210(19) 0.0825(12) Uani 1 1 d . . . F2 F 0.0111(3) -0.2354(3) 0.3530(2) 0.0771(10) Uani 1 1 d . . . F3 F -0.0791(2) -0.0802(3) 0.39814(18) 0.0539(7) Uani 1 1 d . . . F4 F -0.2037(3) 0.3396(4) 0.1851(3) 0.0820(11) Uani 1 1 d . . . F5 F -0.2822(2) 0.1436(4) 0.1746(2) 0.0694(9) Uani 1 1 d . . . F6 F -0.2287(2) 0.2279(4) 0.07018(18) 0.0727(10) 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 0.02938(18) 0.0365(2) 0.03343(19) 0.00200(13) 0.00583(12) -0.00121(12) Si1 0.0314(6) 0.0344(6) 0.0319(6) 0.0066(5) 0.0018(5) 0.0054(5) Si2 0.0295(5) 0.0276(5) 0.0282(6) 0.0021(4) 0.0007(4) 0.0007(4) O1 0.0283(14) 0.0401(16) 0.0327(15) 0.0035(13) 0.0038(12) -0.0001(12) O2 0.0373(16) 0.0379(16) 0.0399(16) 0.0068(13) 0.0076(13) 0.0065(13) C1 0.033(2) 0.033(2) 0.033(2) 0.0023(17) 0.0033(17) -0.0039(17) C2 0.030(2) 0.031(2) 0.033(2) 0.0001(17) 0.0034(16) -0.0023(17) C3 0.065(3) 0.057(3) 0.040(3) 0.001(2) -0.011(2) 0.018(3) C4 0.044(3) 0.063(3) 0.056(3) 0.014(3) 0.013(2) 0.018(2) C5 0.044(3) 0.037(2) 0.064(3) 0.012(2) 0.006(2) 0.006(2) C6 0.048(3) 0.036(2) 0.066(3) -0.010(2) -0.001(2) 0.009(2) C7 0.051(3) 0.057(3) 0.041(3) 0.013(2) 0.013(2) 0.000(2) C8 0.038(2) 0.045(3) 0.038(2) -0.001(2) -0.0050(19) -0.0012(19) C9 0.031(2) 0.046(3) 0.036(2) 0.0039(19) 0.0033(17) 0.0018(18) C10 0.031(2) 0.029(2) 0.029(2) -0.0051(16) -0.0007(16) -0.0035(16) C11 0.0275(19) 0.042(2) 0.029(2) -0.0044(17) 0.0067(16) -0.0019(16) C12 0.032(2) 0.0293(19) 0.030(2) -0.0054(16) 0.0014(16) 0.0041(16) C13 0.040(2) 0.049(3) 0.037(2) 0.005(2) 0.0050(19) 0.008(2) F1 0.0493(18) 0.150(4) 0.0397(17) 0.0278(19) -0.0123(13) -0.0307(19) F2 0.116(3) 0.0468(18) 0.078(2) 0.0242(16) 0.043(2) 0.0201(18) F3 0.0444(15) 0.074(2) 0.0456(16) 0.0197(14) 0.0153(13) 0.0097(13) F4 0.066(2) 0.060(2) 0.112(3) -0.019(2) -0.0056(19) 0.0312(17) F5 0.0312(14) 0.092(2) 0.084(2) 0.0351(19) 0.0070(14) 0.0100(15) F6 0.0481(16) 0.127(3) 0.0400(16) 0.0186(18) 0.0000(13) 0.0309(18) _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 O1 2.245(3) . ? Ag1 O2 2.251(3) . ? Ag1 C2 2.255(4) . ? Ag1 C1 2.267(4) . ? Si1 C4 1.846(5) . ? Si1 C3 1.853(5) . ? Si1 C5 1.856(5) . ? Si1 C1 1.877(4) . ? Si2 C6 1.847(5) . ? Si2 C7 1.848(4) . ? Si2 C8 1.860(4) . ? Si2 C2 1.868(4) . ? O1 C10 1.246(5) . ? O2 C12 1.246(5) . ? C1 C2 1.222(6) . ? C9 F1 1.311(5) . ? C9 F3 1.325(5) . ? C9 F2 1.329(5) . ? C9 C10 1.535(6) . ? C10 C11 1.396(6) . ? C11 C12 1.403(6) . ? C12 C13 1.543(6) . ? C13 F6 1.312(5) . ? C13 F5 1.323(5) . ? C13 F4 1.331(6) . ? 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 O1 Ag1 O2 83.30(10) . . ? O1 Ag1 C2 157.73(12) . . ? O2 Ag1 C2 118.97(12) . . ? O1 Ag1 C1 126.42(12) . . ? O2 Ag1 C1 150.14(13) . . ? C2 Ag1 C1 31.37(14) . . ? C4 Si1 C3 111.4(3) . . ? C4 Si1 C5 112.3(3) . . ? C3 Si1 C5 111.8(3) . . ? C4 Si1 C1 107.9(2) . . ? C3 Si1 C1 107.9(2) . . ? C5 Si1 C1 105.13(19) . . ? C6 Si2 C7 112.1(2) . . ? C6 Si2 C8 110.8(2) . . ? C7 Si2 C8 112.0(2) . . ? C6 Si2 C2 108.8(2) . . ? C7 Si2 C2 106.4(2) . . ? C8 Si2 C2 106.55(19) . . ? C10 O1 Ag1 126.7(3) . . ? C12 O2 Ag1 125.7(3) . . ? C2 C1 Si1 173.6(4) . . ? C2 C1 Ag1 73.8(3) . . ? Si1 C1 Ag1 111.91(19) . . ? C1 C2 Si2 170.8(4) . . ? C1 C2 Ag1 74.9(3) . . ? Si2 C2 Ag1 113.86(18) . . ? F1 C9 F3 107.4(4) . . ? F1 C9 F2 106.9(4) . . ? F3 C9 F2 105.3(4) . . ? F1 C9 C10 111.2(4) . . ? F3 C9 C10 114.8(3) . . ? F2 C9 C10 110.9(4) . . ? O1 C10 C11 129.6(4) . . ? O1 C10 C9 113.5(3) . . ? C11 C10 C9 116.9(4) . . ? C10 C11 C12 124.0(4) . . ? O2 C12 C11 130.1(4) . . ? O2 C12 C13 113.1(4) . . ? C11 C12 C13 116.6(4) . . ? F6 C13 F5 107.3(4) . . ? F6 C13 F4 107.2(4) . . ? F5 C13 F4 106.0(4) . . ? F6 C13 C12 111.9(4) . . ? F5 C13 C12 113.6(4) . . ? F4 C13 C12 110.4(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 O2 Ag1 O1 C10 1.8(3) . . . . ? C2 Ag1 O1 C10 -178.3(3) . . . . ? C1 Ag1 O1 C10 -175.0(3) . . . . ? O1 Ag1 O2 C12 -7.1(3) . . . . ? C2 Ag1 O2 C12 173.0(3) . . . . ? C1 Ag1 O2 C12 167.7(3) . . . . ? C4 Si1 C1 C2 15(3) . . . . ? C3 Si1 C1 C2 135(3) . . . . ? C5 Si1 C1 C2 -106(3) . . . . ? C4 Si1 C1 Ag1 165.6(2) . . . . ? C3 Si1 C1 Ag1 -73.9(3) . . . . ? C5 Si1 C1 Ag1 45.5(3) . . . . ? O1 Ag1 C1 C2 -177.6(2) . . . . ? O2 Ag1 C1 C2 8.8(4) . . . . ? O1 Ag1 C1 Si1 5.6(3) . . . . ? O2 Ag1 C1 Si1 -167.93(17) . . . . ? C2 Ag1 C1 Si1 -176.8(4) . . . . ? Si1 C1 C2 Si2 -9(5) . . . . ? Ag1 C1 C2 Si2 -162(2) . . . . ? Si1 C1 C2 Ag1 152(3) . . . . ? C6 Si2 C2 C1 -130(2) . . . . ? C7 Si2 C2 C1 -10(2) . . . . ? C8 Si2 C2 C1 110(2) . . . . ? C6 Si2 C2 Ag1 69.1(3) . . . . ? C7 Si2 C2 Ag1 -170.0(2) . . . . ? C8 Si2 C2 Ag1 -50.4(2) . . . . ? O1 Ag1 C2 C1 5.1(5) . . . . ? O2 Ag1 C2 C1 -175.0(2) . . . . ? O1 Ag1 C2 Si2 -178.1(2) . . . . ? O2 Ag1 C2 Si2 1.8(3) . . . . ? C1 Ag1 C2 Si2 176.8(4) . . . . ? Ag1 O1 C10 C11 3.2(6) . . . . ? Ag1 O1 C10 C9 -177.3(2) . . . . ? F1 C9 C10 O1 51.3(5) . . . . ? F3 C9 C10 O1 173.4(4) . . . . ? F2 C9 C10 O1 -67.4(5) . . . . ? F1 C9 C10 C11 -129.1(4) . . . . ? F3 C9 C10 C11 -7.0(5) . . . . ? F2 C9 C10 C11 112.2(4) . . . . ? O1 C10 C11 C12 -4.9(7) . . . . ? C9 C10 C11 C12 175.5(4) . . . . ? Ag1 O2 C12 C11 8.4(6) . . . . ? Ag1 O2 C12 C13 -175.8(3) . . . . ? C10 C11 C12 O2 -1.8(7) . . . . ? C10 C11 C12 C13 -177.5(4) . . . . ? O2 C12 C13 F6 35.9(5) . . . . ? C11 C12 C13 F6 -147.7(4) . . . . ? O2 C12 C13 F5 157.6(4) . . . . ? C11 C12 C13 F5 -26.0(6) . . . . ? O2 C12 C13 F4 -83.5(5) . . . . ? C11 C12 C13 F4 92.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.946 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.118