#------------------------------------------------------------------------------ #$Date: 2024-07-05 18:35:15 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292979 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248658.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7248658 loop_ _publ_author_name 'Ward, Jas S.' _publ_section_title ; The atypical solubility of silver(i) pentafluorobenzoate and its use as a catch-and-release agent ; _journal_issue 23 _journal_name_full CrystEngComm _journal_page_first 3088 _journal_page_last 3097 _journal_paper_doi 10.1039/D4CE00441H _journal_volume 26 _journal_year 2024 _chemical_formula_moiety '2(C13 H6 Ag F5 O2)' _chemical_formula_sum 'C26 H12 Ag2 F10 O4' _chemical_formula_weight 794.10 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-10-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-11-24 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _cell_angle_alpha 105.107(3) _cell_angle_beta 90.214(2) _cell_angle_gamma 90.163(2) _cell_formula_units_Z 2 _cell_length_a 5.69188(13) _cell_length_b 12.5817(3) _cell_length_c 17.9282(6) _cell_measurement_reflns_used 7885 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 75.6340 _cell_measurement_theta_min 3.6120 _cell_volume 1239.51(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -4.00 24.00 0.50 0.40 -- -51.70 19.00-180.00 56 2 \w -53.00 -17.00 0.50 1.40 -- -87.58 57.00-180.00 72 3 \w -77.00 -32.00 0.50 0.40 -- -51.70 84.00-120.00 90 4 \w -93.00 -68.00 0.50 1.40 -- -87.58 84.00-120.00 50 5 \w -26.00 5.00 0.50 0.40 -- -51.70 84.00-120.00 62 6 \w -4.00 25.00 0.50 0.40 -- -51.70 19.00 -30.00 58 7 \w 94.00 172.00 0.50 1.40 -- 102.12 38.00-180.00 156 8 \w 101.00 169.00 0.50 1.40 -- 102.12 77.00-150.00 136 9 \w 91.00 156.00 0.50 1.40 -- 102.12 84.00-120.00 130 10 \w 28.00 78.00 0.50 1.40 -- 102.12 -57.00 120.00 100 11 \w 44.00 97.00 0.50 1.40 -- 102.12 -77.00 0.00 106 12 \w 32.00 68.00 0.50 1.40 -- 102.12 -57.00 30.00 72 13 \w 44.00 71.00 0.50 1.40 -- 102.12 -57.00 0.00 54 14 \w 26.00 52.00 0.50 1.40 -- 102.12 -38.00 -60.00 52 15 \w 42.00 67.00 0.50 1.40 -- 102.12 -57.00 -90.00 50 16 \w 44.00 69.00 0.50 1.40 -- 102.12 -57.00-150.00 50 17 \w 49.00 97.00 0.50 1.40 -- 102.12 -77.00-180.00 96 18 \w 29.00 78.00 0.50 1.40 -- 102.12 -57.00-180.00 98 19 \w 25.00 50.00 0.50 1.40 -- 102.12 -38.00 90.00 50 20 \w 41.00 107.00 0.50 1.40 -- 102.12 -84.00 119.00 132 21 \w 54.00 80.00 0.50 0.40 -- 51.89 -84.00 119.00 52 22 \w -9.00 31.00 0.50 0.40 -- 51.89 -84.00 119.00 80 23 \w -120.00 -74.00 0.50 0.40 -- -51.70-125.00 90.00 92 24 \w -120.00 -80.00 0.50 0.40 -- -51.70-125.00 60.00 80 25 \w -111.00 -79.00 0.50 1.40 -- -87.58 -84.00 119.00 64 26 \w -152.00-117.00 0.50 1.40 -- -87.58 -84.00 119.00 70 27 \w -119.00 -74.00 0.50 0.40 -- -51.70-125.00 -90.00 90 28 \w 122.00 147.00 0.50 1.40 -- 102.12 76.00 131.00 50 29 \w -27.00 23.00 0.50 0.40 -- -51.89 38.00 90.00 100 30 \w 101.00 126.00 0.50 0.40 -- 52.14 57.00 -30.00 50 31 \w 41.00 93.00 0.50 0.40 -- 52.14 57.00 -30.00 104 32 \w -100.00 -75.00 0.50 1.40 -- -87.58-125.00 -30.00 50 33 \w -50.00 -17.00 0.50 1.40 -- -87.58 57.00 60.00 66 34 \w -153.00-124.00 0.50 1.40 -- -87.58-125.00 -30.00 58 35 \w 56.00 109.00 0.50 1.40 -- 94.00-113.00 45.25 106 36 \w 59.00 121.00 0.50 1.40 -- 98.00-137.00 12.08 124 37 \w 78.00 104.00 0.50 1.40 -- 102.12 -99.00 120.00 52 38 \w 80.00 106.00 0.50 1.40 -- 102.12 -99.00-180.00 52 39 \w 59.00 85.00 0.50 1.40 -- 102.12-125.00 -60.00 52 40 \w 43.00 74.00 0.50 1.40 -- 102.12 -99.00 120.00 62 41 \w 59.00 106.00 0.50 1.40 -- 102.12 -99.00 90.00 94 42 \w 133.00 173.00 0.50 1.40 -- 102.12 19.00 120.00 80 43 \w 26.00 52.00 0.50 1.40 -- 102.12 -38.00 0.00 52 44 \w 81.00 106.00 0.50 1.40 -- 102.12 -99.00-120.00 50 45 \w 71.00 100.00 0.50 1.40 -- 102.12 -99.00 0.00 58 46 \w 76.00 102.00 0.50 1.40 -- 102.12 -99.00-150.00 52 47 \w 37.00 63.00 0.50 1.40 -- 102.12 -57.00 -60.00 52 48 \w 49.00 75.00 0.50 1.40 -- 102.12 -99.00 30.00 52 49 \w 80.00 106.00 0.50 1.40 -- 102.12 -99.00 30.00 52 50 \w 33.00 68.00 0.50 1.40 -- 102.12-125.00 -30.00 70 51 \w 74.00 106.00 0.50 1.40 -- 102.12-125.00 -30.00 64 52 \w 138.00 164.00 0.50 1.40 -- 102.12 77.00 0.00 52 53 \w 25.00 50.00 0.50 1.40 -- 102.12 -38.00 -30.00 50 54 \w 26.00 51.00 0.50 1.40 -- 102.12 -38.00 -90.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix-Arc 100' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.2382010000 _diffrn_orient_matrix_UB_12 -0.0344739000 _diffrn_orient_matrix_UB_13 0.0270770000 _diffrn_orient_matrix_UB_21 0.0026037000 _diffrn_orient_matrix_UB_22 0.1033439000 _diffrn_orient_matrix_UB_23 0.0687155000 _diffrn_orient_matrix_UB_31 -0.1285005000 _diffrn_orient_matrix_UB_32 0.0649397000 _diffrn_orient_matrix_UB_33 -0.0496710000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_unetI/netI 0.0407 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 18171 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.496 _diffrn_reflns_theta_min 2.553 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.706 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.128 _exptl_crystal_description needle _exptl_crystal_F_000 768 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: benzene/pentane' _exptl_crystal_size_max 0.126 _exptl_crystal_size_mid 0.014 _exptl_crystal_size_min 0.008 _refine_diff_density_max 1.912 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.127 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 379 _refine_ls_number_reflns 5044 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.148 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0440 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+7.0258P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.1091 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4271 _reflns_number_total 5044 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_Benzene _cod_depositor_comments 'Adding full bibliography for 7248652--7248666.cif.' _cod_database_code 7248658 _shelxl_version_number 2014/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.898 _shelx_estimated_absorpt_t_min 0.277 _diffrn_oxdiff_digest_frames ; 014cd19d042dd1f6fee729ab7e624cd67c0395231d6 ; _diffrn_oxdiff_digest_hkl ; 01fc4b5cdac3e41c132ae0e7a53e46a7b42dd6 ; _reflns_odcompleteness_completeness 99.49 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C111(H111), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116) ; _shelx_res_file ; TITL ohd491_3_test_a.res in P-1 REM Old TITL OHD491_3_test in P-1 REM SHELXT solution in P-1: R1 0.193, Rweak 0.022, Alpha 0.062 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C26 O3 F11 Ag2 CELL 1.54184 5.691876 12.581697 17.928158 105.1072 90.2144 90.1633 ZERR 2 0.000132 0.00034 0.000553 0.0025 0.0022 0.002 LATT 1 SFAC C H Ag F O UNIT 52 24 4 20 8 L.S. 4 PLAN 5 SIZE 0.008 0.014 0.126 TEMP -153.15 BIND C102 Ag1 BIND C111 Ag2 BIND C112 Ag2 bond $H list 4 fmap 2 acta SHEL 50 0.8 REM REM REM WGHT 0.024300 7.025800 FVAR 2.82677 AG1 3 0.296106 0.555677 0.985538 11.00000 0.01465 0.04097 = 0.04858 0.02899 -0.00002 -0.00392 AG2 3 -0.204569 0.063340 0.505149 11.00000 0.01603 0.02515 = 0.06444 -0.00346 0.00123 -0.00388 F20 4 0.709186 0.870486 0.961410 11.00000 0.03335 0.02968 = 0.05757 0.01447 0.01951 0.00724 F21 4 1.009720 0.997616 0.907011 11.00000 0.05179 0.02318 = 0.06520 0.01922 0.01165 -0.00285 F22 4 1.365958 0.904556 0.812700 11.00000 0.03551 0.04406 = 0.05275 0.02783 0.00523 -0.01421 F23 4 1.410467 0.682256 0.767950 11.00000 0.02758 0.04689 = 0.04004 0.01689 0.01354 0.00254 F24 4 1.117833 0.553818 0.824893 11.00000 0.02871 0.02482 = 0.03464 0.00662 0.00392 0.00126 F40 4 0.167159 0.404980 0.527591 11.00000 0.02892 0.03059 = 0.05716 0.01635 -0.01019 0.00188 F41 4 0.441962 0.581318 0.584615 11.00000 0.04893 0.02297 = 0.05989 0.01610 0.00053 -0.00149 F42 4 0.824359 0.565076 0.672789 11.00000 0.04309 0.02950 = 0.04735 0.00381 -0.00072 -0.01899 F43 4 0.923785 0.372771 0.706064 11.00000 0.02502 0.04063 = 0.03568 0.00555 -0.00861 -0.00960 F44 4 0.642301 0.196795 0.653724 11.00000 0.02427 0.02505 = 0.03939 0.01073 -0.00358 -0.00209 O11 5 0.540997 0.639764 0.924588 11.00000 0.00933 0.03741 = 0.04490 0.02339 -0.00284 -0.00434 O13 5 0.868863 0.582228 0.971807 11.00000 0.01980 0.02995 = 0.03900 0.02084 -0.00371 -0.00326 O31 5 0.038720 0.199967 0.558291 11.00000 0.01195 0.02538 = 0.04464 0.00063 -0.00053 -0.00449 O33 5 0.369838 0.106206 0.518705 11.00000 0.01668 0.01935 = 0.04571 -0.00166 0.00351 -0.00553 C12 1 0.757999 0.637777 0.934036 11.00000 0.01810 0.02189 = 0.02612 0.00832 0.00096 0.00094 C14 1 0.907344 0.708678 0.896119 11.00000 0.01719 0.02527 = 0.02886 0.01152 -0.00330 -0.00474 C15 1 0.882113 0.821801 0.914614 11.00000 0.02177 0.02293 = 0.03511 0.01019 0.00402 0.00128 C16 1 1.033417 0.887468 0.886504 11.00000 0.03331 0.02599 = 0.03761 0.01588 -0.00064 -0.00404 C17 1 1.215540 0.840638 0.838527 11.00000 0.02307 0.03247 = 0.03735 0.01973 -0.00237 -0.00793 C18 1 1.239642 0.727889 0.816751 11.00000 0.01785 0.03692 = 0.02716 0.01108 0.00104 -0.00177 C19 1 1.087056 0.663991 0.846070 11.00000 0.01974 0.02471 = 0.02751 0.01020 -0.00445 0.00100 C32 1 0.256633 0.190493 0.550977 11.00000 0.01799 0.02268 = 0.03159 0.00668 0.00156 0.00148 C34 1 0.401374 0.293432 0.586549 11.00000 0.01690 0.01824 = 0.02944 0.00321 0.00365 -0.00068 C35 1 0.352762 0.393623 0.572111 11.00000 0.01647 0.02922 = 0.03423 0.00795 0.00133 0.00076 C36 1 0.492637 0.484763 0.600793 11.00000 0.03559 0.01963 = 0.03694 0.01040 0.00605 0.00285 C37 1 0.684970 0.477922 0.645335 11.00000 0.02851 0.02152 = 0.03246 0.00381 0.00376 -0.00991 C38 1 0.735991 0.379715 0.661929 11.00000 0.01872 0.02762 = 0.02859 0.00320 -0.00112 -0.00719 C39 1 0.592799 0.288972 0.633673 11.00000 0.01647 0.02103 = 0.03252 0.00616 0.00220 -0.00389 C101 1 0.246069 0.669442 1.131468 11.00000 0.03779 0.03756 = 0.03947 -0.00154 0.01494 -0.00771 AFIX 43 H101 2 0.115034 0.620998 1.125721 11.00000 -1.20000 AFIX 0 C102 1 0.232272 0.763029 1.105190 11.00000 0.02965 0.04181 = 0.04498 0.00128 0.00481 0.00051 AFIX 43 H102 2 0.093177 0.778204 1.080442 11.00000 -1.20000 AFIX 0 C103 1 0.422745 0.835221 1.115025 11.00000 0.03874 0.02858 = 0.04611 0.00691 0.00565 0.00009 AFIX 43 H103 2 0.414257 0.899083 1.096240 11.00000 -1.20000 AFIX 0 C104 1 0.621672 0.814439 1.151603 11.00000 0.02617 0.03888 = 0.05013 0.00693 0.00714 -0.00862 AFIX 43 H104 2 0.749299 0.865043 1.159742 11.00000 -1.20000 AFIX 0 C105 1 0.637261 0.719663 1.176802 11.00000 0.03556 0.04824 = 0.04210 0.01226 0.00225 0.00374 AFIX 43 H105 2 0.776532 0.704674 1.201541 11.00000 -1.20000 AFIX 0 C106 1 0.448428 0.646051 1.165890 11.00000 0.05454 0.02979 = 0.03814 0.00604 0.01961 0.00023 AFIX 43 H106 2 0.459883 0.580191 1.182181 11.00000 -1.20000 AFIX 0 C111 1 -0.240119 0.034963 0.350241 11.00000 0.03484 0.05464 = 0.06224 0.03242 -0.01738 -0.02015 AFIX 43 H111 2 -0.371631 -0.006771 0.359017 11.00000 -1.20000 AFIX 0 C112 1 -0.245099 0.147750 0.373826 11.00000 0.03255 0.05367 = 0.04434 0.02358 0.00074 -0.00140 AFIX 43 H112 2 -0.379547 0.183996 0.399649 11.00000 -1.20000 AFIX 0 C113 1 -0.056442 0.208763 0.360307 11.00000 0.03700 0.04252 = 0.05051 0.01991 -0.00788 -0.00388 AFIX 43 H113 2 -0.060225 0.286844 0.377289 11.00000 -1.20000 AFIX 0 C114 1 0.136730 0.156849 0.322362 11.00000 0.02623 0.05923 = 0.05339 0.02674 -0.00302 -0.00492 AFIX 43 H114 2 0.265798 0.198973 0.312234 11.00000 -1.20000 AFIX 0 C115 1 0.143987 0.042104 0.298578 11.00000 0.03976 0.06752 = 0.04955 0.01752 -0.00433 0.01702 AFIX 43 H115 2 0.277643 0.005941 0.272154 11.00000 -1.20000 AFIX 0 C116 1 -0.042200 -0.018047 0.313486 11.00000 0.07606 0.02987 = 0.05999 0.00959 -0.03429 -0.00045 AFIX 43 H116 2 -0.036148 -0.096190 0.298682 11.00000 -1.20000 AFIX 0 HKLF 4 REM ohd491_3_test_a.res in P-1 REM R1 = 0.0440 for 4271 Fo > 4sig(Fo) and 0.0532 for all 5044 data REM 379 parameters refined using 0 restraints END WGHT 0.0244 7.0223 REM Highest difference peak 1.912, deepest hole -1.392, 1-sigma level 0.127 Q1 1 -0.2363 0.0600 0.5603 11.00000 0.05 1.91 Q2 1 0.3109 0.4951 0.9445 11.00000 0.05 1.33 Q3 1 -0.1665 0.0015 0.4688 11.00000 0.05 0.91 Q4 1 0.2977 0.6387 1.0277 11.00000 0.05 0.70 Q5 1 -0.1687 0.0749 0.4409 11.00000 0.05 0.69 ; _shelx_res_checksum 87862 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.249 _oxdiff_exptl_absorpt_empirical_full_min 0.708 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.29611(7) 0.55568(4) 0.98554(3) 0.03151(13) Uani 1 1 d . . . . . Ag2 Ag -0.20457(7) 0.06334(4) 0.50515(3) 0.03803(15) Uani 1 1 d . . . . . F20 F 0.7092(6) 0.8705(3) 0.9614(2) 0.0396(9) Uani 1 1 d . . . . . F21 F 1.0097(7) 0.9976(3) 0.9070(2) 0.0453(10) Uani 1 1 d . . . . . F22 F 1.3660(7) 0.9046(3) 0.8127(2) 0.0413(9) Uani 1 1 d . . . . . F23 F 1.4105(6) 0.6823(3) 0.7680(2) 0.0371(8) Uani 1 1 d . . . . . F24 F 1.1178(6) 0.5538(3) 0.82489(19) 0.0296(7) Uani 1 1 d . . . . . F40 F 0.1672(6) 0.4050(3) 0.5276(2) 0.0380(8) Uani 1 1 d . . . . . F41 F 0.4420(7) 0.5813(3) 0.5846(2) 0.0429(9) Uani 1 1 d . . . . . F42 F 0.8244(7) 0.5651(3) 0.6728(2) 0.0412(9) Uani 1 1 d . . . . . F43 F 0.9238(6) 0.3728(3) 0.7061(2) 0.0346(8) Uani 1 1 d . . . . . F44 F 0.6423(6) 0.1968(3) 0.65372(19) 0.0291(7) Uani 1 1 d . . . . . O11 O 0.5410(6) 0.6398(3) 0.9246(2) 0.0282(9) Uani 1 1 d . . . . . O13 O 0.8689(6) 0.5822(3) 0.9718(2) 0.0274(8) Uani 1 1 d . . . . . O31 O 0.0387(6) 0.2000(3) 0.5583(2) 0.0289(9) Uani 1 1 d . . . . . O33 O 0.3698(6) 0.1062(3) 0.5187(2) 0.0291(9) Uani 1 1 d . . . . . C12 C 0.7580(9) 0.6378(4) 0.9340(3) 0.0216(10) Uani 1 1 d . . . . . C14 C 0.9073(9) 0.7087(4) 0.8961(3) 0.0230(11) Uani 1 1 d . . . . . C15 C 0.8821(10) 0.8218(5) 0.9146(3) 0.0261(11) Uani 1 1 d . . . . . C16 C 1.0334(11) 0.8875(5) 0.8865(4) 0.0309(13) Uani 1 1 d . . . . . C17 C 1.2155(10) 0.8406(5) 0.8385(4) 0.0290(12) Uani 1 1 d . . . . . C18 C 1.2396(9) 0.7279(5) 0.8168(3) 0.0268(12) Uani 1 1 d . . . . . C19 C 1.0871(9) 0.6640(4) 0.8461(3) 0.0234(11) Uani 1 1 d . . . . . C32 C 0.2566(9) 0.1905(4) 0.5510(3) 0.0242(11) Uani 1 1 d . . . . . C34 C 0.4014(9) 0.2934(4) 0.5865(3) 0.0221(10) Uani 1 1 d . . . . . C35 C 0.3528(9) 0.3936(5) 0.5721(3) 0.0267(12) Uani 1 1 d . . . . . C36 C 0.4926(11) 0.4848(5) 0.6008(4) 0.0301(12) Uani 1 1 d . . . . . C37 C 0.6850(10) 0.4779(5) 0.6453(3) 0.0281(12) Uani 1 1 d . . . . . C38 C 0.7360(9) 0.3797(5) 0.6619(3) 0.0258(11) Uani 1 1 d . . . . . C39 C 0.5928(9) 0.2890(4) 0.6337(3) 0.0235(11) Uani 1 1 d . . . . . C101 C 0.2461(12) 0.6694(6) 1.1315(4) 0.0404(15) Uani 1 1 d . . . . . H101 H 0.1150 0.6210 1.1257 0.048 Uiso 1 1 calc R . . . . C102 C 0.2323(12) 0.7630(6) 1.1052(4) 0.0407(15) Uani 1 1 d . . . . . H102 H 0.0932 0.7782 1.0804 0.049 Uiso 1 1 calc R . . . . C103 C 0.4227(12) 0.8352(5) 1.1150(4) 0.0383(14) Uani 1 1 d . . . . . H103 H 0.4143 0.8991 1.0962 0.046 Uiso 1 1 calc R . . . . C104 C 0.6217(11) 0.8144(6) 1.1516(4) 0.0393(15) Uani 1 1 d . . . . . H104 H 0.7493 0.8650 1.1597 0.047 Uiso 1 1 calc R . . . . C105 C 0.6373(12) 0.7197(6) 1.1768(4) 0.0419(15) Uani 1 1 d . . . . . H105 H 0.7765 0.7047 1.2015 0.050 Uiso 1 1 calc R . . . . C106 C 0.4484(13) 0.6461(5) 1.1659(4) 0.0413(16) Uani 1 1 d . . . . . H106 H 0.4599 0.5802 1.1822 0.050 Uiso 1 1 calc R . . . . C111 C -0.2401(13) 0.0350(6) 0.3502(5) 0.0475(18) Uani 1 1 d . . . . . H111 H -0.3716 -0.0068 0.3590 0.057 Uiso 1 1 calc R . . . . C112 C -0.2451(12) 0.1478(6) 0.3738(4) 0.0415(16) Uani 1 1 d . . . . . H112 H -0.3795 0.1840 0.3996 0.050 Uiso 1 1 calc R . . . . C113 C -0.0564(12) 0.2088(6) 0.3603(4) 0.0419(16) Uani 1 1 d . . . . . H113 H -0.0602 0.2868 0.3773 0.050 Uiso 1 1 calc R . . . . C114 C 0.1367(12) 0.1568(7) 0.3224(4) 0.0441(17) Uani 1 1 d . . . . . H114 H 0.2658 0.1990 0.3122 0.053 Uiso 1 1 calc R . . . . C115 C 0.1440(14) 0.0421(7) 0.2986(5) 0.0518(19) Uani 1 1 d . . . . . H115 H 0.2776 0.0059 0.2722 0.062 Uiso 1 1 calc R . . . . C116 C -0.0422(16) -0.0180(6) 0.3135(5) 0.056(2) Uani 1 1 d . . . . . H116 H -0.0361 -0.0962 0.2987 0.067 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01465(19) 0.0410(3) 0.0486(3) 0.0290(2) -0.00002(16) -0.00392(16) Ag2 0.0160(2) 0.0251(2) 0.0644(3) -0.0035(2) 0.00123(19) -0.00388(15) F20 0.0333(19) 0.0297(18) 0.058(2) 0.0145(17) 0.0195(17) 0.0072(15) F21 0.052(2) 0.0232(18) 0.065(3) 0.0192(17) 0.0117(19) -0.0028(16) F22 0.036(2) 0.044(2) 0.053(2) 0.0278(18) 0.0052(16) -0.0142(16) F23 0.0276(18) 0.047(2) 0.040(2) 0.0169(17) 0.0135(15) 0.0025(15) F24 0.0287(17) 0.0248(16) 0.0346(18) 0.0066(14) 0.0039(14) 0.0013(13) F40 0.0289(18) 0.0306(18) 0.057(2) 0.0164(16) -0.0102(16) 0.0019(14) F41 0.049(2) 0.0230(18) 0.060(3) 0.0161(17) 0.0005(18) -0.0015(16) F42 0.043(2) 0.0295(19) 0.047(2) 0.0038(16) -0.0007(17) -0.0190(16) F43 0.0250(17) 0.041(2) 0.0357(19) 0.0056(15) -0.0086(14) -0.0096(14) F44 0.0243(16) 0.0250(16) 0.0394(19) 0.0107(14) -0.0036(13) -0.0021(13) O11 0.0093(17) 0.037(2) 0.045(2) 0.0234(19) -0.0028(15) -0.0043(15) O13 0.0198(19) 0.030(2) 0.039(2) 0.0208(18) -0.0037(16) -0.0033(15) O31 0.0120(18) 0.025(2) 0.045(2) 0.0006(17) -0.0005(16) -0.0045(14) O33 0.0167(18) 0.0193(19) 0.046(2) -0.0017(17) 0.0035(16) -0.0055(14) C12 0.018(3) 0.022(3) 0.026(3) 0.008(2) 0.001(2) 0.0009(19) C14 0.017(2) 0.025(3) 0.029(3) 0.012(2) -0.003(2) -0.005(2) C15 0.022(3) 0.023(3) 0.035(3) 0.010(2) 0.004(2) 0.001(2) C16 0.033(3) 0.026(3) 0.038(3) 0.016(2) -0.001(2) -0.004(2) C17 0.023(3) 0.032(3) 0.037(3) 0.020(3) -0.002(2) -0.008(2) C18 0.018(3) 0.037(3) 0.027(3) 0.011(2) 0.001(2) -0.002(2) C19 0.020(3) 0.025(3) 0.028(3) 0.010(2) -0.004(2) 0.001(2) C32 0.018(3) 0.023(3) 0.032(3) 0.007(2) 0.002(2) 0.001(2) C34 0.017(2) 0.018(2) 0.029(3) 0.003(2) 0.004(2) -0.0007(19) C35 0.016(3) 0.029(3) 0.034(3) 0.008(2) 0.001(2) 0.001(2) C36 0.036(3) 0.020(3) 0.037(3) 0.010(2) 0.006(2) 0.003(2) C37 0.029(3) 0.022(3) 0.032(3) 0.004(2) 0.004(2) -0.010(2) C38 0.019(3) 0.028(3) 0.029(3) 0.003(2) -0.001(2) -0.007(2) C39 0.016(2) 0.021(3) 0.033(3) 0.006(2) 0.002(2) -0.0039(19) C101 0.038(4) 0.038(4) 0.039(4) -0.002(3) 0.015(3) -0.008(3) C102 0.030(3) 0.042(4) 0.045(4) 0.001(3) 0.005(3) 0.001(3) C103 0.039(4) 0.029(3) 0.046(4) 0.007(3) 0.006(3) 0.000(3) C104 0.026(3) 0.039(4) 0.050(4) 0.007(3) 0.007(3) -0.009(3) C105 0.036(4) 0.048(4) 0.042(4) 0.012(3) 0.002(3) 0.004(3) C106 0.055(4) 0.030(3) 0.038(4) 0.006(3) 0.020(3) 0.000(3) C111 0.035(4) 0.055(4) 0.062(5) 0.032(4) -0.017(3) -0.020(3) C112 0.033(3) 0.054(4) 0.044(4) 0.024(3) 0.001(3) -0.001(3) C113 0.037(4) 0.043(4) 0.051(4) 0.020(3) -0.008(3) -0.004(3) C114 0.026(3) 0.059(5) 0.053(4) 0.027(4) -0.003(3) -0.005(3) C115 0.040(4) 0.068(5) 0.050(4) 0.018(4) -0.004(3) 0.017(4) C116 0.076(6) 0.030(4) 0.060(5) 0.010(3) -0.034(4) 0.000(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 5 8 0.0022 0 -5 -8 0.0062 0 -6 10 0.0086 0 6 -10 0.0046 4 0 -1 0.0537 -4 0 1 0.0717 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 Ag1 Ag1 C102 111.09(14) 2_667 . ? O11 Ag1 Ag1 84.02(10) . 2_667 ? O11 Ag1 O13 159.16(15) . 2_667 ? O11 Ag1 O13 118.53(13) . 1_455 ? O11 Ag1 C101 110.79(19) . . ? O11 Ag1 C102 89.65(18) . . ? O13 Ag1 Ag1 155.61(9) 1_455 2_667 ? O13 Ag1 Ag1 79.57(9) 2_667 2_667 ? O13 Ag1 O13 76.30(14) 2_667 1_455 ? O13 Ag1 C101 83.38(18) 2_667 . ? O13 Ag1 C101 86.29(19) 1_455 . ? O13 Ag1 C102 108.16(18) 2_667 . ? O13 Ag1 C102 80.14(17) 1_455 . ? C101 Ag1 Ag1 94.44(16) . 2_667 ? C101 Ag1 C102 28.0(2) . . ? Ag2 Ag2 C112 109.94(15) 2_556 . ? O31 Ag2 Ag2 82.83(10) . 2_556 ? O31 Ag2 O33 157.63(15) . 2_556 ? O31 Ag2 O33 116.14(13) . 1_455 ? O31 Ag2 C111 111.38(18) . . ? O31 Ag2 C112 89.41(19) . . ? O33 Ag2 Ag2 157.59(9) 1_455 2_556 ? O33 Ag2 Ag2 80.75(10) 2_556 2_556 ? O33 Ag2 O33 77.64(14) 2_556 1_455 ? O33 Ag2 C111 89.93(19) 1_455 . ? O33 Ag2 C111 84.92(19) 2_556 . ? O33 Ag2 C112 110.43(19) 2_556 . ? O33 Ag2 C112 83.39(17) 1_455 . ? C111 Ag2 Ag2 94.03(17) . 2_556 ? C111 Ag2 C112 28.5(2) . . ? C12 O11 Ag1 122.0(3) . . ? Ag1 O13 Ag1 103.70(14) 2_667 1_655 ? C12 O13 Ag1 123.6(3) . 2_667 ? C12 O13 Ag1 130.7(3) . 1_655 ? C32 O31 Ag2 122.0(4) . . ? Ag2 O33 Ag2 102.36(14) 2_556 1_655 ? C32 O33 Ag2 121.1(3) . 2_556 ? C32 O33 Ag2 133.6(3) . 1_655 ? O11 C12 O13 127.0(5) . . ? O11 C12 C14 117.3(4) . . ? O13 C12 C14 115.7(4) . . ? C15 C14 C12 121.4(5) . . ? C15 C14 C19 117.0(5) . . ? C19 C14 C12 121.4(5) . . ? F20 C15 C14 120.3(5) . . ? F20 C15 C16 118.1(5) . . ? C16 C15 C14 121.6(5) . . ? F21 C16 C15 120.6(5) . . ? F21 C16 C17 119.4(5) . . ? C15 C16 C17 120.0(5) . . ? F22 C17 C16 120.1(5) . . ? F22 C17 C18 120.2(5) . . ? C18 C17 C16 119.7(5) . . ? F23 C18 C17 119.7(5) . . ? F23 C18 C19 121.1(5) . . ? C17 C18 C19 119.2(5) . . ? F24 C19 C14 119.7(5) . . ? F24 C19 C18 117.8(5) . . ? C18 C19 C14 122.5(5) . . ? O31 C32 C34 116.2(5) . . ? O33 C32 O31 127.6(5) . . ? O33 C32 C34 116.2(5) . . ? C35 C34 C32 122.1(5) . . ? C35 C34 C39 117.2(5) . . ? C39 C34 C32 120.7(5) . . ? F40 C35 C34 120.7(5) . . ? F40 C35 C36 117.5(5) . . ? C36 C35 C34 121.7(5) . . ? F41 C36 C35 120.2(5) . . ? F41 C36 C37 119.6(5) . . ? C37 C36 C35 120.2(5) . . ? F42 C37 C36 121.0(5) . . ? F42 C37 C38 119.5(5) . . ? C36 C37 C38 119.5(5) . . ? F43 C38 C37 119.7(5) . . ? F43 C38 C39 120.4(5) . . ? C37 C38 C39 119.9(5) . . ? F44 C39 C34 120.5(5) . . ? F44 C39 C38 118.0(5) . . ? C38 C39 C34 121.4(5) . . ? Ag1 C101 H101 79.3 . . ? C102 C101 Ag1 87.6(4) . . ? C102 C101 H101 119.9 . . ? C106 C101 Ag1 103.0(4) . . ? C106 C101 H101 119.9 . . ? C106 C101 C102 120.3(6) . . ? Ag1 C102 H102 90.8 . . ? C101 C102 Ag1 64.4(4) . . ? C101 C102 H102 120.1 . . ? C101 C102 C103 119.9(7) . . ? C103 C102 Ag1 114.7(4) . . ? C103 C102 H102 120.1 . . ? C102 C103 H103 119.9 . . ? C104 C103 C102 120.2(6) . . ? C104 C103 H103 119.9 . . ? C103 C104 H104 120.0 . . ? C103 C104 C105 120.0(6) . . ? C105 C104 H104 120.0 . . ? C104 C105 H105 120.0 . . ? C104 C105 C106 120.0(7) . . ? C106 C105 H105 120.0 . . ? C101 C106 C105 119.6(6) . . ? C101 C106 H106 120.2 . . ? C105 C106 H106 120.2 . . ? Ag2 C111 H111 79.4 . . ? C112 C111 Ag2 80.6(5) . . ? C112 C111 H111 120.1 . . ? C112 C111 C116 119.8(7) . . ? C116 C111 Ag2 110.3(5) . . ? C116 C111 H111 120.1 . . ? Ag2 C112 H112 84.0 . . ? C111 C112 Ag2 70.9(4) . . ? C111 C112 H112 119.8 . . ? C111 C112 C113 120.4(7) . . ? C113 C112 Ag2 115.6(5) . . ? C113 C112 H112 119.8 . . ? C112 C113 H113 120.0 . . ? C114 C113 C112 120.0(7) . . ? C114 C113 H113 120.0 . . ? C113 C114 H114 120.0 . . ? C113 C114 C115 120.0(7) . . ? C115 C114 H114 120.0 . . ? C114 C115 H115 120.2 . . ? C116 C115 C114 119.7(7) . . ? C116 C115 H115 120.2 . . ? C111 C116 H116 120.0 . . ? C115 C116 C111 120.1(7) . . ? C115 C116 H116 120.0 . . ? 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 Ag1 2.8297(8) 2_667 ? Ag1 O11 2.205(4) . ? Ag1 O13 2.273(4) 2_667 ? Ag1 O13 2.476(4) 1_455 ? Ag1 C101 2.652(6) . ? Ag1 C102 2.938(7) . ? Ag2 Ag2 2.8051(9) 2_556 ? Ag2 O31 2.214(4) . ? Ag2 O33 2.482(4) 1_455 ? Ag2 O33 2.265(4) 2_556 ? Ag2 C111 2.713(8) . ? Ag2 C112 2.833(6) . ? F20 C15 1.338(6) . ? F21 C16 1.345(7) . ? F22 C17 1.337(6) . ? F23 C18 1.337(6) . ? F24 C19 1.350(6) . ? F40 C35 1.352(6) . ? F41 C36 1.352(6) . ? F42 C37 1.336(6) . ? F43 C38 1.344(6) . ? F44 C39 1.331(6) . ? O11 C12 1.247(6) . ? O13 Ag1 2.476(4) 1_655 ? O13 Ag1 2.273(4) 2_667 ? O13 C12 1.261(6) . ? O31 C32 1.250(6) . ? O33 Ag2 2.482(4) 1_655 ? O33 Ag2 2.265(4) 2_556 ? O33 C32 1.250(6) . ? C12 C14 1.515(7) . ? C14 C15 1.383(8) . ? C14 C19 1.384(8) . ? C15 C16 1.376(8) . ? C16 C17 1.381(9) . ? C17 C18 1.377(8) . ? C18 C19 1.377(8) . ? C32 C34 1.524(7) . ? C34 C35 1.380(8) . ? C34 C39 1.386(8) . ? C35 C36 1.378(8) . ? C36 C37 1.369(9) . ? C37 C38 1.376(8) . ? C38 C39 1.384(7) . ? C101 H101 0.9500 . ? C101 C102 1.380(10) . ? C101 C106 1.373(11) . ? C102 H102 0.9500 . ? C102 C103 1.393(9) . ? C103 H103 0.9500 . ? C103 C104 1.366(10) . ? C104 H104 0.9500 . ? C104 C105 1.384(10) . ? C105 H105 0.9500 . ? C105 C106 1.396(10) . ? C106 H106 0.9500 . ? C111 H111 0.9500 . ? C111 C112 1.371(11) . ? C111 C116 1.389(12) . ? C112 H112 0.9500 . ? C112 C113 1.377(9) . ? C113 H113 0.9500 . ? C113 C114 1.370(10) . ? C114 H114 0.9500 . ? C114 C115 1.395(11) . ? C115 H115 0.9500 . ? C115 C116 1.368(12) . ? C116 H116 0.9500 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0946 4.5794 7.5956 0.0253 0.9954 -0.0921 -0.0946 -4.5794 -7.5956 -0.0253 -0.9954 0.0921 -0.0478 -6.0841 9.7533 0.4852 0.0413 -0.8734 0.0478 6.0841 -9.7533 -0.4852 -0.0413 0.8734 3.6832 -0.2382 -0.7965 -0.8907 -0.0698 -0.4492 -3.6832 0.2382 0.7965 0.8907 0.0698 0.4492