#------------------------------------------------------------------------------ #$Date: 2024-05-21 01:38:30 +0300 (Tue, 21 May 2024) $ #$Revision: 291962 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248663.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_7248663 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_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00441H _journal_year 2024 _chemical_formula_moiety '2(C21 H8 Ag2 F10 O4)' _chemical_formula_sum 'C42 H16 Ag4 F20 O8' _chemical_formula_weight 1460.03 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-10-26 _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 90 _cell_angle_beta 97.194(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.60970(10) _cell_length_b 55.4509(15) _cell_length_c 13.6451(4) _cell_measurement_reflns_used 12622 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 76.6640 _cell_measurement_theta_min 3.6180 _cell_volume 4211.07(18) _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)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.01(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 0.996 _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 57.00 113.00 0.50 0.50 -- 42.17 161.00 -65.00 112 2 \w -3.00 22.00 0.50 0.50 -- 46.00 100.00 35.28 50 3 \w 2.00 28.00 0.50 0.50 -- 50.00 96.00 -34.58 52 4 \w 4.00 41.00 0.50 0.50 -- 46.00 86.00 -58.16 74 5 \w 12.00 42.00 0.50 0.50 -- 50.00 82.00-121.76 60 6 \w 15.00 40.00 0.50 0.50 -- 58.00 88.00-146.41 50 7 \w 87.00 157.00 0.50 1.20 -- 113.05 45.00-180.00 140 8 \w 104.00 130.00 0.50 1.20 -- 113.05 161.00 -65.00 52 9 \w 113.00 139.00 0.50 1.20 -- 113.05 118.00 142.00 52 10 \w 112.00 175.00 0.50 1.20 -- 113.05 45.00 60.00 126 11 \w 87.00 171.00 0.50 1.20 -- 113.05 45.00 30.00 168 12 \w 28.00 53.00 0.50 1.20 -- 113.05 -45.00 -90.00 50 13 \w 36.00 61.00 0.50 1.20 -- 113.05 -45.00-120.00 50 14 \w 86.00 111.00 0.50 1.20 -- 113.05-125.00-180.00 50 15 \w 64.00 89.00 0.50 1.20 -- 113.05-161.00 -95.00 50 16 \w 39.00 110.00 0.50 1.20 -- 113.05-125.00 -90.00 142 17 \w 38.00 129.00 0.50 0.50 -- 42.17-161.00 -95.00 182 18 \w 63.00 106.00 0.50 1.20 -- 113.05-118.00 56.00 86 19 \w 32.00 104.00 0.50 1.20 -- 113.05 -95.00 60.00 144 20 \w 40.00 81.00 0.50 1.20 -- 113.05 -95.00 90.00 82 21 \w 33.00 59.00 0.50 1.20 -- 113.05 -45.00 60.00 52 22 \w 33.00 99.00 0.50 1.20 -- 113.05 -95.00 -90.00 132 23 \w 15.00 102.00 0.50 0.50 -- 42.17-118.00 56.00 174 24 \w -101.00 -75.00 0.50 1.20 -- -89.35 118.00 142.00 52 25 \w -59.00 -20.00 0.50 1.20 -- -89.35 61.00 120.00 78 26 \w -60.00 -31.00 0.50 1.20 -- -89.35 61.00 90.00 58 27 \w -37.00 -5.00 0.50 1.20 -- -89.35 45.00 -30.00 64 28 \w -37.00 -12.00 0.50 1.20 -- -89.35 45.00 -60.00 50 29 \w -135.00 -38.00 0.50 1.20 -- -89.35 161.00 -65.00 194 30 \w -130.00 -31.00 0.50 0.50 -- -41.73 161.00 -65.00 198 31 \w -37.00 -6.00 0.50 1.20 -- -89.35 45.00-120.00 62 32 \w -37.00 -9.00 0.50 1.20 -- -89.35 45.00 -90.00 56 33 \w -33.00 -5.00 0.50 1.20 -- -89.35 45.00 0.00 56 34 \w -149.00 -38.00 0.50 0.50 -- -70.00 -63.00 74.20 222 35 \w -129.00 -92.00 0.50 1.20 -- -89.35-118.00 56.00 74 36 \w -124.00 -54.00 0.50 0.50 -- -41.73-178.00 60.00 140 37 \w -156.00 -50.00 0.50 1.20 -- -89.35-161.00 -95.00 212 38 \w -113.00 -51.00 0.50 0.50 -- -41.73-161.00 -95.00 124 ; _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 -0.1395552000 _diffrn_orient_matrix_UB_12 0.0043321000 _diffrn_orient_matrix_UB_13 0.0887180000 _diffrn_orient_matrix_UB_21 0.0137664000 _diffrn_orient_matrix_UB_22 -0.0271164000 _diffrn_orient_matrix_UB_23 0.0243698000 _diffrn_orient_matrix_UB_31 0.2386614000 _diffrn_orient_matrix_UB_32 0.0041110000 _diffrn_orient_matrix_UB_33 0.0671110000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_unetI/netI 0.0489 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 69 _diffrn_reflns_limit_k_min -63 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 43475 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.504 _diffrn_reflns_theta_min 3.188 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 16.051 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_correction_T_min 0.207 _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 2.303 _exptl_crystal_description needle _exptl_crystal_F_000 2800 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: toluene/pentane' _exptl_crystal_size_max 0.123 _exptl_crystal_size_mid 0.027 _exptl_crystal_size_min 0.011 _refine_diff_density_max 0.848 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.135 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 669 _refine_ls_number_reflns 8525 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0528 _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^)+(0.0518P)^2^+19.3420P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1267 _refine_ls_wR_factor_ref 0.1333 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6833 _reflns_number_total 8525 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_Toluene _cod_database_code 7248663 _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 0.843 _shelx_estimated_absorpt_t_min 0.243 _diffrn_oxdiff_digest_frames ; 013280eb7686c27c7a1edf228fa3b87075037709371 ; _diffrn_oxdiff_digest_hkl ; 0175935cb213e272576273ff4812688659f960 ; _reflns_odcompleteness_completeness 99.43 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116) 2.b Idealised Me refined as rotating group: C107(H10A,H10B,H10C), C117(H11A,H11B,H11C) ; _shelx_res_file ; TITL ohd491_9_numabs2_a.res in P2(1)/n REM Old TITL OHD491_9_numabs2 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.226, Rweak 0.018, Alpha 0.065, Orientation as input REM Formula found by SHELXT: C42 O8 F20 Ag4 CELL 1.54184 5.6097 55.4509 13.6451 90 97.194 90 ZERR 4 0.0001 0.0015 0.0004 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ag F O UNIT 168 64 16 80 32 L.S. 4 0 0 PLAN 20 SIZE 0.011 0.027 0.123 TEMP -153.15 BIND Ag3 C114 FREE C115 Ag4 BOND $H list 4 fmap 2 53 ACTA SHEL 50 0.8 REM REM REM WGHT 0.051800 19.342001 FVAR 0.13679 AG1 3 -0.037655 0.730447 0.260061 11.00000 0.02764 0.03534 = 0.04983 -0.00047 0.00572 0.00328 AG2 3 0.381642 0.759496 0.309442 11.00000 0.02685 0.03520 = 0.06102 -0.00055 0.00679 0.00310 AG3 3 0.218461 0.985583 0.515549 11.00000 0.02868 0.03225 = 0.09333 -0.00851 0.01969 -0.00420 AG4 3 0.710879 0.987547 0.020828 11.00000 0.02650 0.04421 = 0.16898 0.04136 0.01449 -0.00115 F20 4 -0.506020 0.791227 0.135253 11.00000 0.05977 0.06517 = 0.04335 -0.00769 -0.00414 0.02189 F21 4 -0.803411 0.829213 0.120949 11.00000 0.06553 0.08088 = 0.04877 0.01147 -0.00320 0.03586 F22 4 -0.708120 0.867627 0.243451 11.00000 0.05186 0.04273 = 0.09823 0.01689 0.02475 0.02022 F23 4 -0.310543 0.867683 0.376956 11.00000 0.05074 0.04109 = 0.15614 -0.03075 -0.00069 0.00447 F24 4 -0.010256 0.829833 0.392730 11.00000 0.03840 0.05000 = 0.12736 -0.03305 -0.02219 0.00120 F40 4 0.357707 0.657077 0.207288 11.00000 0.05213 0.05427 = 0.14124 -0.03895 -0.03208 0.00985 F41 4 0.657844 0.619413 0.241511 11.00000 0.06555 0.03927 = 0.15551 -0.02921 -0.01332 0.00809 F42 4 1.065477 0.623693 0.368168 11.00000 0.05135 0.04168 = 0.09693 0.01151 0.01953 0.01604 F43 4 1.155883 0.665313 0.471094 11.00000 0.06021 0.06904 = 0.05895 0.00738 -0.01368 0.02037 F44 4 0.855680 0.702481 0.440663 11.00000 0.06418 0.05393 = 0.04065 -0.01101 -0.00881 0.01499 F60 4 -0.140054 0.919482 0.617632 11.00000 0.04013 0.04191 = 0.07667 0.01065 -0.01881 -0.00400 F61 4 -0.417062 0.880100 0.626440 11.00000 0.06430 0.04621 = 0.11151 0.03272 -0.02238 -0.01074 F62 4 -0.820249 0.874534 0.496274 11.00000 0.05371 0.03678 = 0.12686 0.01456 -0.02237 -0.01919 F63 4 -0.944315 0.908201 0.355346 11.00000 0.04123 0.04967 = 0.06471 -0.00443 -0.01280 -0.00729 F64 4 -0.670399 0.947884 0.346691 11.00000 0.04331 0.04594 = 0.04168 0.00484 0.00527 -0.00012 F80 4 0.312037 0.912699 -0.039347 11.00000 0.04772 0.04092 = 0.06535 -0.00183 0.02764 -0.00310 F81 4 0.052590 0.874064 -0.002393 11.00000 0.05716 0.03412 = 0.06871 -0.00568 0.01874 -0.00599 F82 4 -0.285881 0.877387 0.121928 11.00000 0.05297 0.04285 = 0.07190 0.01147 0.01712 -0.01524 F83 4 -0.350845 0.919393 0.216789 11.00000 0.03630 0.06437 = 0.05176 0.00857 0.01709 0.00208 F84 4 -0.077443 0.958206 0.186145 11.00000 0.03683 0.04599 = 0.05961 -0.00930 0.00685 0.00271 O11 5 -0.196338 0.767125 0.280914 11.00000 0.02759 0.02944 = 0.04732 -0.00058 0.00718 0.00129 O13 5 0.132509 0.790055 0.283486 11.00000 0.02274 0.03283 = 0.08705 0.00608 0.01125 0.00474 O31 5 0.213631 0.700011 0.293130 11.00000 0.02494 0.03424 = 0.06956 0.00213 0.00818 -0.00050 O33 5 0.540981 0.722988 0.290906 11.00000 0.02780 0.03341 = 0.04351 -0.00190 0.00907 0.00083 O51 5 -0.039375 0.956305 0.474647 11.00000 0.02146 0.03572 = 0.07398 -0.00985 0.01541 -0.00126 O53 5 -0.368525 0.977294 0.498726 11.00000 0.02286 0.03103 = 0.06840 0.00036 0.01316 -0.00058 O71 5 0.479142 0.957358 0.049229 11.00000 0.02309 0.03499 = 0.06450 0.00526 0.00596 -0.00388 O73 5 0.132683 0.977490 0.019427 11.00000 0.02763 0.03334 = 0.09722 0.01577 0.00521 -0.00308 C12 1 -0.090049 0.786897 0.278162 11.00000 0.02808 0.03765 = 0.03758 0.00080 0.00991 -0.00056 C14 1 -0.249046 0.809086 0.264826 11.00000 0.03168 0.03102 = 0.04755 0.00682 0.01330 0.00397 C15 1 -0.452453 0.809839 0.195027 11.00000 0.03810 0.04479 = 0.03822 0.00572 0.01174 0.00969 C16 1 -0.607028 0.829284 0.187503 11.00000 0.04497 0.05427 = 0.04289 0.01738 0.01781 0.01308 C17 1 -0.560471 0.848680 0.249279 11.00000 0.03806 0.04019 = 0.07480 0.01893 0.02710 0.00886 C18 1 -0.356740 0.848696 0.317693 11.00000 0.04105 0.02937 = 0.09259 -0.00893 0.01118 -0.00158 C19 1 -0.202890 0.829580 0.323487 11.00000 0.03004 0.03675 = 0.08430 -0.00208 0.00627 -0.00337 C32 1 0.436409 0.703056 0.298679 11.00000 0.03403 0.03279 = 0.03807 -0.00079 0.00779 0.00182 C34 1 0.596204 0.681279 0.320405 11.00000 0.02906 0.03484 = 0.05135 -0.00139 0.01667 0.00087 C35 1 0.552375 0.659456 0.272804 11.00000 0.03522 0.03818 = 0.07789 -0.00965 0.00007 -0.00059 C36 1 0.708394 0.640144 0.287957 11.00000 0.05260 0.03272 = 0.09217 -0.00969 0.01292 -0.00151 C37 1 0.911330 0.642448 0.354022 11.00000 0.03821 0.04278 = 0.06440 0.01361 0.01965 0.00853 C38 1 0.958179 0.663155 0.406151 11.00000 0.04406 0.04453 = 0.05073 0.01068 0.01463 0.00735 C39 1 0.802096 0.682423 0.388661 11.00000 0.03838 0.03842 = 0.04020 0.01137 0.00955 0.00722 C52 1 -0.256988 0.958043 0.484839 11.00000 0.03698 0.02629 = 0.04077 -0.00458 0.00335 -0.00098 C54 1 -0.401313 0.935134 0.483120 11.00000 0.01980 0.02878 = 0.04929 -0.00562 0.00206 -0.00177 C55 1 -0.338107 0.917029 0.551399 11.00000 0.03101 0.03505 = 0.05965 0.00168 -0.00060 0.00240 C56 1 -0.479737 0.896915 0.557448 11.00000 0.03897 0.02940 = 0.07924 0.00972 -0.01036 -0.00430 C57 1 -0.684438 0.894140 0.491563 11.00000 0.03557 0.03481 = 0.07796 -0.00205 0.00143 -0.00719 C58 1 -0.747711 0.911281 0.420533 11.00000 0.03499 0.03541 = 0.05113 -0.00608 -0.00032 0.00059 C59 1 -0.605634 0.931427 0.417128 11.00000 0.02836 0.03527 = 0.04188 -0.00129 0.00667 -0.00028 C72 1 0.256071 0.958986 0.044594 11.00000 0.02634 0.03234 = 0.05071 0.00362 0.00935 -0.00511 C74 1 0.120995 0.936792 0.070824 11.00000 0.02803 0.03396 = 0.03818 0.00750 0.00091 -0.00173 C75 1 0.151954 0.914878 0.025688 11.00000 0.02956 0.03673 = 0.04399 0.00723 0.00819 0.00222 C76 1 0.019612 0.894993 0.043587 11.00000 0.03144 0.03210 = 0.04711 0.00155 0.00140 -0.00101 C77 1 -0.152741 0.896631 0.107077 11.00000 0.03112 0.03700 = 0.04692 0.01177 0.00537 -0.00525 C78 1 -0.184152 0.917939 0.154209 11.00000 0.02709 0.04773 = 0.04010 0.00763 0.00681 0.00233 C79 1 -0.048009 0.937692 0.136880 11.00000 0.02612 0.03873 = 0.04268 -0.00024 0.00740 -0.00180 C101 1 0.452874 0.795115 0.540096 11.00000 0.05589 0.05013 = 0.03460 0.00270 -0.00607 0.00205 C102 1 0.620104 0.780888 0.502570 11.00000 0.03896 0.07098 = 0.04114 0.00207 0.00076 -0.00734 AFIX 43 H102 2 0.754666 0.788333 0.479173 11.00000 -1.20000 AFIX 0 C103 1 0.598700 0.755994 0.497759 11.00000 0.04362 0.07183 = 0.04663 -0.00973 0.00105 0.01049 AFIX 43 H103 2 0.717724 0.746529 0.472093 11.00000 -1.20000 AFIX 0 C104 1 0.400790 0.745079 0.530988 11.00000 0.06236 0.04886 = 0.04935 0.00357 -0.00337 -0.00133 AFIX 43 H104 2 0.381573 0.728070 0.527162 11.00000 -1.20000 AFIX 0 C105 1 0.231556 0.759230 0.569787 11.00000 0.03749 0.07754 = 0.05165 0.01588 0.00595 0.00021 AFIX 43 H105 2 0.096892 0.751936 0.593704 11.00000 -1.20000 AFIX 0 C106 1 0.259975 0.784304 0.573562 11.00000 0.04582 0.07447 = 0.04504 -0.00113 0.00257 0.01564 AFIX 43 H106 2 0.143173 0.793947 0.599828 11.00000 -1.20000 AFIX 0 C107 1 0.479870 0.822096 0.543417 11.00000 0.09071 0.06151 = 0.07343 -0.00638 -0.02155 0.00286 AFIX 137 H10A 2 0.649231 0.826351 0.542791 11.00000 -1.50000 H10B 2 0.424368 0.828303 0.603880 11.00000 -1.50000 H10C 2 0.383602 0.829216 0.485743 11.00000 -1.50000 AFIX 0 C111 1 0.559583 0.956446 0.792117 11.00000 0.05320 0.04654 = 0.05281 0.00378 0.01594 -0.00692 C112 1 0.331320 0.951158 0.747128 11.00000 0.04980 0.04635 = 0.04912 -0.00005 0.00614 -0.00520 AFIX 43 H112 2 0.281523 0.934803 0.740427 11.00000 -1.20000 AFIX 0 C113 1 0.174711 0.969126 0.711841 11.00000 0.04661 0.06717 = 0.04982 -0.00184 0.00912 -0.00655 AFIX 43 H113 2 0.017914 0.965026 0.681868 11.00000 -1.20000 AFIX 0 C114 1 0.242586 0.993064 0.719440 11.00000 0.06250 0.05020 = 0.05143 0.00321 0.00877 0.00762 AFIX 43 H114 2 0.132266 1.005411 0.696308 11.00000 -1.20000 AFIX 0 C115 1 0.472772 0.998846 0.761070 11.00000 0.06644 0.04893 = 0.04981 -0.00030 0.00852 -0.01208 AFIX 43 H115 2 0.524049 1.015186 0.764139 11.00000 -1.20000 AFIX 0 C116 1 0.629956 0.980569 0.798656 11.00000 0.04686 0.06606 = 0.04729 0.00219 0.00308 -0.01636 AFIX 43 H116 2 0.786521 0.984632 0.829004 11.00000 -1.20000 AFIX 0 C117 1 0.725563 0.936734 0.836218 11.00000 0.05515 0.06326 = 0.07288 0.01877 0.01210 -0.00090 AFIX 137 H11A 2 0.696370 0.933734 0.904485 11.00000 -1.50000 H11B 2 0.892822 0.941747 0.835387 11.00000 -1.50000 H11C 2 0.695138 0.921939 0.797383 11.00000 -1.50000 AFIX 0 HKLF 4 REM ohd491_9_numabs2_a.res in P2(1)/n REM R1 = 0.0528 for 6833 Fo > 4sig(Fo) and 0.0662 for all 8525 data REM 669 parameters refined using 0 restraints END WGHT 0.0518 19.3281 REM Highest difference peak 0.848, deepest hole -0.998, 1-sigma level 0.135 Q1 1 0.3840 0.7389 0.3064 11.00000 0.05 0.85 Q2 1 0.3779 0.7604 0.2560 11.00000 0.05 0.78 Q3 1 0.3105 0.7598 0.2444 11.00000 0.05 0.78 Q4 1 -0.3824 0.7601 0.2791 11.00000 0.05 0.71 Q5 1 -0.0227 0.7379 0.2389 11.00000 0.05 0.69 Q6 1 0.1882 0.7326 0.2574 11.00000 0.05 0.64 Q7 1 0.5077 0.9876 0.0364 11.00000 0.05 0.64 Q8 1 0.1810 0.9796 0.4385 11.00000 0.05 0.62 Q9 1 0.8250 0.9800 0.1056 11.00000 0.05 0.62 Q10 1 -0.0309 0.7004 0.2620 11.00000 0.05 0.60 Q11 1 0.3785 0.7773 0.3177 11.00000 0.05 0.58 Q12 1 0.0032 0.9971 0.5188 11.00000 0.05 0.57 Q13 1 0.6904 1.0044 0.0635 11.00000 0.05 0.55 Q14 1 -0.2416 0.9819 0.4670 11.00000 0.05 0.54 Q15 1 0.2046 1.0056 0.5279 11.00000 0.05 0.54 Q16 1 0.9014 0.9988 0.0013 11.00000 0.05 0.53 Q17 1 0.2860 0.9800 -0.0241 11.00000 0.05 0.52 Q18 1 0.3503 0.6586 0.1384 11.00000 0.05 0.51 Q19 1 0.2296 0.9588 0.5160 11.00000 0.05 0.51 Q20 1 -0.0734 0.9788 0.4599 11.00000 0.05 0.50 ; _shelx_res_checksum 19932 _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 1.566 _oxdiff_exptl_absorpt_empirical_full_min 0.657 loop_ _space_group_symop_operation_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' 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 -0.03766(8) 0.73045(2) 0.26006(4) 0.03753(13) Uani 1 1 d . . . . . Ag2 Ag 0.38164(8) 0.75950(2) 0.30944(4) 0.04091(13) Uani 1 1 d . . . . . Ag3 Ag 0.21846(9) 0.98558(2) 0.51555(5) 0.05040(16) Uani 1 1 d . . . . . Ag4 Ag 0.71088(10) 0.98755(2) 0.02083(7) 0.0797(3) Uani 1 1 d . . . . . F20 F -0.5060(8) 0.79123(9) 0.1353(3) 0.0570(11) Uani 1 1 d . . . . . F21 F -0.8034(9) 0.82921(10) 0.1209(3) 0.0659(14) Uani 1 1 d . . . . . F22 F -0.7081(8) 0.86763(8) 0.2435(4) 0.0630(13) Uani 1 1 d . . . . . F23 F -0.3105(9) 0.86768(9) 0.3770(5) 0.0838(19) Uani 1 1 d . . . . . F24 F -0.0103(8) 0.82983(8) 0.3927(5) 0.0747(16) Uani 1 1 d . . . . . F40 F 0.3577(9) 0.65708(9) 0.2073(5) 0.086(2) Uani 1 1 d . . . . . F41 F 0.6578(10) 0.61941(9) 0.2415(5) 0.089(2) Uani 1 1 d . . . . . F42 F 1.0655(8) 0.62369(8) 0.3682(4) 0.0625(12) Uani 1 1 d . . . . . F43 F 1.1559(9) 0.66531(9) 0.4711(3) 0.0645(13) Uani 1 1 d . . . . . F44 F 0.8557(8) 0.70248(8) 0.4407(3) 0.0542(11) Uani 1 1 d . . . . . F60 F -0.1401(7) 0.91948(8) 0.6176(4) 0.0551(11) Uani 1 1 d . . . . . F61 F -0.4171(9) 0.88010(9) 0.6264(5) 0.0768(17) Uani 1 1 d . . . . . F62 F -0.8202(9) 0.87453(8) 0.4963(5) 0.0753(17) Uani 1 1 d . . . . . F63 F -0.9443(7) 0.90820(8) 0.3553(3) 0.0535(11) Uani 1 1 d . . . . . F64 F -0.6704(7) 0.94788(7) 0.3467(3) 0.0436(9) Uani 1 1 d . . . . . F80 F 0.3120(7) 0.91270(7) -0.0393(3) 0.0496(10) Uani 1 1 d . . . . . F81 F 0.0526(8) 0.87406(7) -0.0024(3) 0.0524(10) Uani 1 1 d . . . . . F82 F -0.2859(8) 0.87739(8) 0.1219(3) 0.0551(11) Uani 1 1 d . . . . . F83 F -0.3508(7) 0.91939(8) 0.2168(3) 0.0498(10) Uani 1 1 d . . . . . F84 F -0.0774(7) 0.95821(7) 0.1861(3) 0.0474(9) Uani 1 1 d . . . . . O11 O -0.1963(7) 0.76713(8) 0.2809(3) 0.0346(9) Uani 1 1 d . . . . . O13 O 0.1325(8) 0.79005(8) 0.2835(4) 0.0472(12) Uani 1 1 d . . . . . O31 O 0.2136(8) 0.70001(8) 0.2931(4) 0.0427(11) Uani 1 1 d . . . . . O33 O 0.5410(7) 0.72299(8) 0.2909(3) 0.0345(9) Uani 1 1 d . . . . . O51 O -0.0394(7) 0.95631(8) 0.4746(4) 0.0429(11) Uani 1 1 d . . . . . O53 O -0.3685(7) 0.97729(8) 0.4987(4) 0.0401(10) Uani 1 1 d . . . . . O71 O 0.4791(7) 0.95736(8) 0.0492(4) 0.0408(10) Uani 1 1 d . . . . . O73 O 0.1327(8) 0.97749(9) 0.0194(5) 0.0530(14) Uani 1 1 d . . . . . C12 C -0.0900(11) 0.78690(12) 0.2782(5) 0.0339(13) Uani 1 1 d . . . . . C14 C -0.2490(11) 0.80909(11) 0.2648(5) 0.0360(14) Uani 1 1 d . . . . . C15 C -0.4525(12) 0.80984(13) 0.1950(5) 0.0398(15) Uani 1 1 d . . . . . C16 C -0.6070(13) 0.82928(14) 0.1875(5) 0.0463(17) Uani 1 1 d . . . . . C17 C -0.5605(13) 0.84868(13) 0.2493(6) 0.0493(18) Uani 1 1 d . . . . . C18 C -0.3567(14) 0.84870(13) 0.3177(7) 0.054(2) Uani 1 1 d . . . . . C19 C -0.2029(13) 0.82958(13) 0.3235(7) 0.0504(18) Uani 1 1 d . . . . . C32 C 0.4364(11) 0.70306(11) 0.2987(5) 0.0347(13) Uani 1 1 d . . . . . C34 C 0.5962(11) 0.68128(12) 0.3204(5) 0.0374(14) Uani 1 1 d . . . . . C35 C 0.5524(13) 0.65946(14) 0.2728(6) 0.0510(18) Uani 1 1 d . . . . . C36 C 0.7084(15) 0.64014(14) 0.2880(7) 0.059(2) Uani 1 1 d . . . . . C37 C 0.9113(13) 0.64245(13) 0.3540(6) 0.0473(17) Uani 1 1 d . . . . . C38 C 0.9582(13) 0.66315(14) 0.4062(5) 0.0457(16) Uani 1 1 d . . . . . C39 C 0.8021(12) 0.68242(12) 0.3887(5) 0.0386(14) Uani 1 1 d . . . . . C52 C -0.2570(11) 0.95804(11) 0.4848(5) 0.0348(13) Uani 1 1 d . . . . . C54 C -0.4013(10) 0.93513(11) 0.4831(5) 0.0328(13) Uani 1 1 d . . . . . C55 C -0.3381(12) 0.91703(12) 0.5514(6) 0.0424(15) Uani 1 1 d . . . . . C56 C -0.4797(13) 0.89692(12) 0.5574(6) 0.0507(19) Uani 1 1 d . . . . . C57 C -0.6844(13) 0.89414(13) 0.4916(6) 0.0499(18) Uani 1 1 d . . . . . C58 C -0.7477(12) 0.91128(12) 0.4205(5) 0.0410(15) Uani 1 1 d . . . . . C59 C -0.6056(11) 0.93143(12) 0.4171(5) 0.0350(13) Uani 1 1 d . . . . . C72 C 0.2561(11) 0.95899(11) 0.0446(5) 0.0361(14) Uani 1 1 d . . . . . C74 C 0.1210(11) 0.93679(11) 0.0708(5) 0.0337(13) Uani 1 1 d . . . . . C75 C 0.1520(11) 0.91488(12) 0.0257(5) 0.0365(14) Uani 1 1 d . . . . . C76 C 0.0196(11) 0.89499(12) 0.0436(5) 0.0372(14) Uani 1 1 d . . . . . C77 C -0.1527(11) 0.89663(12) 0.1071(5) 0.0383(14) Uani 1 1 d . . . . . C78 C -0.1842(11) 0.91794(13) 0.1542(5) 0.0381(14) Uani 1 1 d . . . . . C79 C -0.0480(11) 0.93769(12) 0.1369(5) 0.0356(13) Uani 1 1 d . . . . . C101 C 0.4529(14) 0.79511(14) 0.5401(5) 0.0479(17) Uani 1 1 d . . . . . C102 C 0.6201(13) 0.78089(16) 0.5026(5) 0.0507(18) Uani 1 1 d . . . . . H102 H 0.7547 0.7883 0.4792 0.061 Uiso 1 1 calc R . . . . C103 C 0.5987(14) 0.75599(16) 0.4978(6) 0.054(2) Uani 1 1 d . . . . . H103 H 0.7177 0.7465 0.4721 0.065 Uiso 1 1 calc R . . . . C104 C 0.4008(15) 0.74508(15) 0.5310(6) 0.0544(19) Uani 1 1 d . . . . . H104 H 0.3816 0.7281 0.5272 0.065 Uiso 1 1 calc R . . . . C105 C 0.2316(14) 0.75923(17) 0.5698(6) 0.056(2) Uani 1 1 d . . . . . H105 H 0.0969 0.7519 0.5937 0.067 Uiso 1 1 calc R . . . . C106 C 0.2600(14) 0.78430(17) 0.5736(6) 0.055(2) Uani 1 1 d . . . . . H106 H 0.1432 0.7939 0.5998 0.066 Uiso 1 1 calc R . . . . C107 C 0.480(2) 0.82210(17) 0.5434(8) 0.078(3) Uani 1 1 d . . . . . H10A H 0.6492 0.8264 0.5428 0.117 Uiso 1 1 calc GR . . . . H10B H 0.4244 0.8283 0.6039 0.117 Uiso 1 1 calc GR . . . . H10C H 0.3836 0.8292 0.4857 0.117 Uiso 1 1 calc GR . . . . C111 C 0.5596(14) 0.95645(14) 0.7921(6) 0.0501(18) Uani 1 1 d . . . . . C112 C 0.3313(14) 0.95116(14) 0.7471(5) 0.0484(17) Uani 1 1 d . . . . . H112 H 0.2815 0.9348 0.7404 0.058 Uiso 1 1 calc R . . . . C113 C 0.1747(15) 0.96913(16) 0.7118(6) 0.0543(19) Uani 1 1 d . . . . . H113 H 0.0179 0.9650 0.6819 0.065 Uiso 1 1 calc R . . . . C114 C 0.2426(15) 0.99306(15) 0.7194(6) 0.0546(19) Uani 1 1 d . . . . . H114 H 0.1323 1.0054 0.6963 0.065 Uiso 1 1 calc R . . . . C115 C 0.4728(15) 0.99885(16) 0.7611(6) 0.0550(19) Uani 1 1 d . . . . . H115 H 0.5240 1.0152 0.7641 0.066 Uiso 1 1 calc R . . . . C116 C 0.6300(14) 0.98057(16) 0.7987(6) 0.0536(19) Uani 1 1 d . . . . . H116 H 0.7865 0.9846 0.8290 0.064 Uiso 1 1 calc R . . . . C117 C 0.7256(15) 0.93673(17) 0.8362(7) 0.063(2) Uani 1 1 d . . . . . H11A H 0.6964 0.9337 0.9045 0.095 Uiso 1 1 calc GR . . . . H11B H 0.8928 0.9417 0.8354 0.095 Uiso 1 1 calc GR . . . . H11C H 0.6951 0.9219 0.7974 0.095 Uiso 1 1 calc GR . . . . 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 0.0276(2) 0.0353(2) 0.0498(3) -0.0005(2) 0.00572(18) 0.00328(18) Ag2 0.0268(2) 0.0352(2) 0.0610(3) -0.0005(2) 0.00679(19) 0.00310(18) Ag3 0.0287(3) 0.0322(3) 0.0933(4) -0.0085(2) 0.0197(2) -0.00420(19) Ag4 0.0265(3) 0.0442(3) 0.1690(8) 0.0414(4) 0.0145(3) -0.0012(2) F20 0.060(3) 0.065(3) 0.043(2) -0.008(2) -0.0041(19) 0.022(2) F21 0.066(3) 0.081(3) 0.049(2) 0.011(2) -0.003(2) 0.036(3) F22 0.052(3) 0.043(2) 0.098(4) 0.017(2) 0.025(2) 0.020(2) F23 0.051(3) 0.041(3) 0.156(6) -0.031(3) -0.001(3) 0.004(2) F24 0.038(2) 0.050(3) 0.127(5) -0.033(3) -0.022(3) 0.001(2) F40 0.052(3) 0.054(3) 0.141(5) -0.039(3) -0.032(3) 0.010(2) F41 0.066(3) 0.039(3) 0.156(6) -0.029(3) -0.013(3) 0.008(2) F42 0.051(3) 0.042(2) 0.097(4) 0.012(2) 0.020(2) 0.016(2) F43 0.060(3) 0.069(3) 0.059(3) 0.007(2) -0.014(2) 0.020(2) F44 0.064(3) 0.054(3) 0.041(2) -0.0110(19) -0.0088(19) 0.015(2) F60 0.040(2) 0.042(2) 0.077(3) 0.011(2) -0.019(2) -0.0040(18) F61 0.064(3) 0.046(3) 0.112(4) 0.033(3) -0.022(3) -0.011(2) F62 0.054(3) 0.037(2) 0.127(5) 0.015(3) -0.022(3) -0.019(2) F63 0.041(2) 0.050(2) 0.065(3) -0.004(2) -0.0128(19) -0.0073(19) F64 0.043(2) 0.046(2) 0.042(2) 0.0048(17) 0.0053(16) -0.0001(17) F80 0.048(2) 0.041(2) 0.065(3) -0.0018(19) 0.028(2) -0.0031(18) F81 0.057(3) 0.034(2) 0.069(3) -0.0057(19) 0.019(2) -0.0060(18) F82 0.053(3) 0.043(2) 0.072(3) 0.011(2) 0.017(2) -0.0152(19) F83 0.036(2) 0.064(3) 0.052(2) 0.009(2) 0.0171(17) 0.0021(19) F84 0.037(2) 0.046(2) 0.060(2) -0.0093(19) 0.0069(17) 0.0027(17) O11 0.028(2) 0.029(2) 0.047(2) -0.0006(18) 0.0072(18) 0.0013(17) O13 0.023(2) 0.033(2) 0.087(4) 0.006(2) 0.011(2) 0.0047(18) O31 0.025(2) 0.034(2) 0.070(3) 0.002(2) 0.008(2) -0.0005(18) O33 0.028(2) 0.033(2) 0.044(2) -0.0019(18) 0.0091(17) 0.0008(18) O51 0.021(2) 0.036(2) 0.074(3) -0.010(2) 0.015(2) -0.0013(18) O53 0.023(2) 0.031(2) 0.068(3) 0.000(2) 0.0132(19) -0.0006(17) O71 0.023(2) 0.035(2) 0.064(3) 0.005(2) 0.0060(19) -0.0039(18) O73 0.028(2) 0.033(3) 0.097(4) 0.016(3) 0.005(2) -0.0031(19) C12 0.028(3) 0.038(3) 0.038(3) 0.001(3) 0.010(2) -0.001(3) C14 0.032(3) 0.031(3) 0.048(4) 0.007(3) 0.013(3) 0.004(3) C15 0.038(4) 0.045(4) 0.038(3) 0.006(3) 0.012(3) 0.010(3) C16 0.045(4) 0.054(4) 0.043(4) 0.017(3) 0.018(3) 0.013(3) C17 0.038(4) 0.040(4) 0.075(5) 0.019(4) 0.027(3) 0.009(3) C18 0.041(4) 0.029(3) 0.093(6) -0.009(4) 0.011(4) -0.002(3) C19 0.030(4) 0.037(4) 0.084(6) -0.002(4) 0.006(3) -0.003(3) C32 0.034(3) 0.033(3) 0.038(3) -0.001(3) 0.008(3) 0.002(3) C34 0.029(3) 0.035(3) 0.051(4) -0.001(3) 0.017(3) 0.001(3) C35 0.035(4) 0.038(4) 0.078(5) -0.010(4) 0.000(3) -0.001(3) C36 0.053(5) 0.033(4) 0.092(6) -0.010(4) 0.013(4) -0.002(3) C37 0.038(4) 0.043(4) 0.064(5) 0.014(3) 0.020(3) 0.009(3) C38 0.044(4) 0.045(4) 0.051(4) 0.011(3) 0.015(3) 0.007(3) C39 0.038(4) 0.038(4) 0.040(3) 0.011(3) 0.010(3) 0.007(3) C52 0.037(4) 0.026(3) 0.041(3) -0.005(2) 0.003(3) -0.001(2) C54 0.020(3) 0.029(3) 0.049(4) -0.006(3) 0.002(2) -0.002(2) C55 0.031(3) 0.035(3) 0.060(4) 0.002(3) -0.001(3) 0.002(3) C56 0.039(4) 0.029(3) 0.079(5) 0.010(3) -0.010(4) -0.004(3) C57 0.036(4) 0.035(4) 0.078(5) -0.002(3) 0.001(3) -0.007(3) C58 0.035(4) 0.035(3) 0.051(4) -0.006(3) 0.000(3) 0.001(3) C59 0.028(3) 0.035(3) 0.042(3) -0.001(3) 0.007(2) 0.000(2) C72 0.026(3) 0.032(3) 0.051(4) 0.004(3) 0.009(3) -0.005(2) C74 0.028(3) 0.034(3) 0.038(3) 0.008(3) 0.001(2) -0.002(2) C75 0.030(3) 0.037(3) 0.044(3) 0.007(3) 0.008(3) 0.002(3) C76 0.031(3) 0.032(3) 0.047(4) 0.002(3) 0.001(3) -0.001(3) C77 0.031(3) 0.037(3) 0.047(4) 0.012(3) 0.005(3) -0.005(3) C78 0.027(3) 0.048(4) 0.040(3) 0.008(3) 0.007(2) 0.002(3) C79 0.026(3) 0.039(3) 0.043(3) 0.000(3) 0.007(2) -0.002(3) C101 0.056(5) 0.050(4) 0.035(3) 0.003(3) -0.006(3) 0.002(3) C102 0.039(4) 0.071(5) 0.041(4) 0.002(4) 0.001(3) -0.007(4) C103 0.044(4) 0.072(6) 0.047(4) -0.010(4) 0.001(3) 0.010(4) C104 0.062(5) 0.049(4) 0.049(4) 0.004(3) -0.003(4) -0.001(4) C105 0.037(4) 0.078(6) 0.052(4) 0.016(4) 0.006(3) 0.000(4) C106 0.046(4) 0.074(6) 0.045(4) -0.001(4) 0.003(3) 0.016(4) C107 0.091(7) 0.062(6) 0.073(6) -0.006(5) -0.022(5) 0.003(5) C111 0.053(5) 0.047(4) 0.053(4) 0.004(3) 0.016(3) -0.007(3) C112 0.050(4) 0.046(4) 0.049(4) 0.000(3) 0.006(3) -0.005(3) C113 0.047(4) 0.067(5) 0.050(4) -0.002(4) 0.009(3) -0.007(4) C114 0.062(5) 0.050(4) 0.051(4) 0.003(4) 0.009(4) 0.008(4) C115 0.066(5) 0.049(4) 0.050(4) 0.000(4) 0.009(4) -0.012(4) C116 0.047(4) 0.066(5) 0.047(4) 0.002(4) 0.003(3) -0.016(4) C117 0.055(5) 0.063(5) 0.073(6) 0.019(4) 0.012(4) -0.001(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 -36 1 0.0102 0 36 -1 0.0012 0 2 9 0.0188 0 -2 -9 0.0078 4 5 -1 0.0598 -4 -5 1 0.0598 1 4 8 0.0309 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 O11 Ag1 Ag2 77.77(11) . . ? O11 Ag1 O33 74.32(15) . 1_455 ? O31 Ag1 Ag2 84.10(12) . . ? O31 Ag1 O11 156.38(17) . . ? O31 Ag1 O33 115.73(16) . 1_455 ? O33 Ag1 Ag2 145.55(10) 1_455 . ? O11 Ag2 Ag1 146.19(10) 1_655 . ? O11 Ag2 C103 80.6(2) 1_655 . ? O13 Ag2 Ag1 84.76(12) . . ? O13 Ag2 O11 116.30(16) . 1_655 ? O13 Ag2 O33 159.02(18) . . ? O13 Ag2 C103 114.2(2) . . ? O33 Ag2 Ag1 78.02(11) . . ? O33 Ag2 O11 74.60(15) . 1_655 ? O33 Ag2 C103 84.5(2) . . ? C103 Ag2 Ag1 116.2(2) . . ? O51 Ag3 Ag3 81.58(12) . 3_576 ? O51 Ag3 O53 153.89(19) . 3_576 ? O51 Ag3 O53 116.50(16) . 1_655 ? O51 Ag3 C114 108.1(2) . . ? O53 Ag3 Ag3 153.59(11) 1_655 3_576 ? O53 Ag3 Ag3 78.55(11) 3_576 3_576 ? O53 Ag3 O53 77.89(17) 3_576 1_655 ? O53 Ag3 C114 101.3(2) 1_655 . ? O53 Ag3 C114 88.8(2) 3_576 . ? C114 Ag3 Ag3 89.91(18) . 3_576 ? O71 Ag4 Ag4 84.57(12) . 3_675 ? O71 Ag4 O73 115.27(16) . 1_655 ? O71 Ag4 O73 166.83(18) . 3_675 ? O73 Ag4 Ag4 82.33(13) 3_675 3_675 ? O73 Ag4 Ag4 158.45(13) 1_655 3_675 ? O73 Ag4 O73 77.51(18) 3_675 1_655 ? Ag1 O11 Ag2 105.40(16) . 1_455 ? C12 O11 Ag1 126.2(4) . . ? C12 O11 Ag2 128.4(4) . 1_455 ? C12 O13 Ag2 120.7(4) . . ? C32 O31 Ag1 121.0(4) . . ? Ag2 O33 Ag1 105.66(17) . 1_655 ? C32 O33 Ag1 128.4(4) . 1_655 ? C32 O33 Ag2 125.9(4) . . ? C52 O51 Ag3 122.4(4) . . ? Ag3 O53 Ag3 102.12(17) 3_576 1_455 ? C52 O53 Ag3 132.7(4) . 1_455 ? C52 O53 Ag3 124.4(4) . 3_576 ? C72 O71 Ag4 123.4(4) . . ? Ag4 O73 Ag4 102.49(18) 3_675 1_455 ? C72 O73 Ag4 133.3(4) . 1_455 ? C72 O73 Ag4 123.8(4) . 3_675 ? O11 C12 O13 126.6(6) . . ? O11 C12 C14 116.0(5) . . ? O13 C12 C14 117.4(6) . . ? C15 C14 C12 121.7(6) . . ? C15 C14 C19 116.4(6) . . ? C19 C14 C12 121.8(6) . . ? F20 C15 C14 120.0(6) . . ? F20 C15 C16 118.1(6) . . ? C16 C15 C14 121.9(7) . . ? F21 C16 C15 120.3(7) . . ? F21 C16 C17 119.8(7) . . ? C17 C16 C15 119.9(7) . . ? F22 C17 C16 120.8(7) . . ? F22 C17 C18 119.6(7) . . ? C16 C17 C18 119.6(7) . . ? F23 C18 C17 119.5(7) . . ? F23 C18 C19 120.4(7) . . ? C19 C18 C17 120.2(7) . . ? F24 C19 C14 119.1(6) . . ? F24 C19 C18 118.7(7) . . ? C18 C19 C14 122.0(7) . . ? O31 C32 O33 125.7(6) . . ? O31 C32 C34 117.8(6) . . ? O33 C32 C34 116.5(5) . . ? C35 C34 C32 122.8(6) . . ? C35 C34 C39 116.0(6) . . ? C39 C34 C32 121.1(6) . . ? F40 C35 C34 119.1(7) . . ? F40 C35 C36 118.4(7) . . ? C34 C35 C36 122.4(7) . . ? F41 C36 C35 120.4(8) . . ? F41 C36 C37 120.5(7) . . ? C37 C36 C35 119.1(7) . . ? F42 C37 C36 119.2(7) . . ? F42 C37 C38 119.8(7) . . ? C38 C37 C36 121.0(7) . . ? F43 C38 C37 120.9(7) . . ? F43 C38 C39 120.0(7) . . ? C37 C38 C39 119.1(7) . . ? F44 C39 C34 120.5(6) . . ? F44 C39 C38 117.2(6) . . ? C38 C39 C34 122.3(7) . . ? O51 C52 O53 126.2(6) . . ? O51 C52 C54 117.7(5) . . ? O53 C52 C54 116.1(6) . . ? C55 C54 C52 120.6(6) . . ? C59 C54 C52 122.5(6) . . ? C59 C54 C55 116.9(6) . . ? F60 C55 C54 119.8(6) . . ? F60 C55 C56 118.3(6) . . ? C56 C55 C54 121.7(6) . . ? F61 C56 C55 120.2(6) . . ? F61 C56 C57 120.4(6) . . ? C57 C56 C55 119.5(7) . . ? F62 C57 C56 119.7(7) . . ? F62 C57 C58 120.0(7) . . ? C58 C57 C56 120.3(7) . . ? F63 C58 C57 120.0(6) . . ? F63 C58 C59 120.9(6) . . ? C57 C58 C59 119.1(6) . . ? F64 C59 C54 119.6(6) . . ? F64 C59 C58 118.0(6) . . ? C58 C59 C54 122.4(6) . . ? O71 C72 O73 125.8(6) . . ? O71 C72 C74 117.3(6) . . ? O73 C72 C74 116.9(5) . . ? C75 C74 C72 121.0(6) . . ? C75 C74 C79 117.0(6) . . ? C79 C74 C72 121.9(6) . . ? F80 C75 C74 120.3(6) . . ? F80 C75 C76 117.9(6) . . ? C76 C75 C74 121.8(6) . . ? F81 C76 C75 120.2(6) . . ? F81 C76 C77 119.9(6) . . ? C75 C76 C77 119.8(6) . . ? F82 C77 C76 119.5(6) . . ? F82 C77 C78 120.9(6) . . ? C78 C77 C76 119.6(6) . . ? F83 C78 C77 119.4(6) . . ? F83 C78 C79 120.5(6) . . ? C77 C78 C79 120.1(6) . . ? F84 C79 C74 119.5(6) . . ? F84 C79 C78 119.0(6) . . ? C78 C79 C74 121.5(6) . . ? C102 C101 C107 120.8(8) . . ? C106 C101 C102 118.7(8) . . ? C106 C101 C107 120.5(9) . . ? C101 C102 H102 119.0 . . ? C101 C102 C103 122.0(8) . . ? C103 C102 H102 119.0 . . ? Ag2 C103 H103 86.7 . . ? C102 C103 Ag2 90.0(5) . . ? C102 C103 H103 120.5 . . ? C102 C103 C104 119.1(8) . . ? C104 C103 Ag2 93.3(5) . . ? C104 C103 H103 120.5 . . ? C103 C104 H104 120.3 . . ? C105 C104 C103 119.4(8) . . ? C105 C104 H104 120.3 . . ? C104 C105 H105 120.1 . . ? C104 C105 C106 119.7(8) . . ? C106 C105 H105 120.1 . . ? C101 C106 C105 121.0(8) . . ? C101 C106 H106 119.5 . . ? C105 C106 H106 119.5 . . ? C101 C107 H10A 109.5 . . ? C101 C107 H10B 109.5 . . ? C101 C107 H10C 109.5 . . ? H10A C107 H10B 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C112 C111 C116 118.1(8) . . ? C112 C111 C117 121.0(7) . . ? C116 C111 C117 120.9(8) . . ? C111 C112 H112 119.4 . . ? C113 C112 C111 121.2(8) . . ? C113 C112 H112 119.4 . . ? C112 C113 H113 119.6 . . ? C112 C113 C114 120.8(8) . . ? C114 C113 H113 119.6 . . ? Ag3 C114 H114 80.1 . . ? C113 C114 Ag3 78.7(5) . . ? C113 C114 H114 120.4 . . ? C113 C114 C115 119.2(8) . . ? C115 C114 Ag3 111.7(5) . . ? C115 C114 H114 120.4 . . ? C114 C115 H115 120.1 . . ? C114 C115 C116 119.8(8) . . ? C116 C115 H115 120.1 . . ? C111 C116 C115 120.8(7) . . ? C111 C116 H116 119.6 . . ? C115 C116 H116 119.6 . . ? C111 C117 H11A 109.5 . . ? C111 C117 H11B 109.5 . . ? C111 C117 H11C 109.5 . . ? H11A C117 H11B 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? 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 Ag2 2.8608(7) . ? Ag1 O11 2.252(4) . ? Ag1 O31 2.209(5) . ? Ag1 O33 2.487(4) 1_455 ? Ag2 O11 2.483(4) 1_655 ? Ag2 O13 2.197(4) . ? Ag2 O33 2.240(4) . ? Ag2 C103 2.709(8) . ? Ag3 Ag3 2.9126(10) 3_576 ? Ag3 O51 2.199(4) . ? Ag3 O53 2.401(4) 1_655 ? Ag3 O53 2.242(4) 3_576 ? Ag3 C114 2.799(8) . ? Ag4 Ag4 2.7370(11) 3_675 ? Ag4 O71 2.184(4) . ? Ag4 O73 2.433(5) 1_655 ? Ag4 O73 2.225(5) 3_675 ? F20 C15 1.326(8) . ? F21 C16 1.337(9) . ? F22 C17 1.334(8) . ? F23 C18 1.333(9) . ? F24 C19 1.343(9) . ? F40 C35 1.328(9) . ? F41 C36 1.326(9) . ? F42 C37 1.351(8) . ? F43 C38 1.335(9) . ? F44 C39 1.333(8) . ? F60 C55 1.348(8) . ? F61 C56 1.340(9) . ? F62 C57 1.334(8) . ? F63 C58 1.338(8) . ? F64 C59 1.342(7) . ? F80 C75 1.345(7) . ? F81 C76 1.343(8) . ? F82 C77 1.332(7) . ? F83 C78 1.345(7) . ? F84 C79 1.342(8) . ? O11 Ag2 2.483(4) 1_455 ? O11 C12 1.251(8) . ? O13 C12 1.254(8) . ? O31 C32 1.254(8) . ? O33 Ag1 2.487(4) 1_655 ? O33 C32 1.262(8) . ? O51 C52 1.250(8) . ? O53 Ag3 2.401(4) 1_455 ? O53 Ag3 2.242(4) 3_576 ? O53 C52 1.264(8) . ? O71 C72 1.248(8) . ? O73 Ag4 2.225(5) 3_675 ? O73 Ag4 2.433(5) 1_455 ? O73 C72 1.261(8) . ? C12 C14 1.517(9) . ? C14 C15 1.392(9) . ? C14 C19 1.395(10) . ? C15 C16 1.379(10) . ? C16 C17 1.371(12) . ? C17 C18 1.382(11) . ? C18 C19 1.363(10) . ? C32 C34 1.511(9) . ? C34 C35 1.381(10) . ? C34 C39 1.391(9) . ? C35 C36 1.382(11) . ? C36 C37 1.367(12) . ? C37 C38 1.359(11) . ? C38 C39 1.383(9) . ? C52 C54 1.505(8) . ? C54 C55 1.385(9) . ? C54 C59 1.381(8) . ? C55 C56 1.378(10) . ? C56 C57 1.375(10) . ? C57 C58 1.372(11) . ? C58 C59 1.376(9) . ? C72 C74 1.512(8) . ? C74 C75 1.383(9) . ? C74 C79 1.388(9) . ? C75 C76 1.368(9) . ? C76 C77 1.380(10) . ? C77 C78 1.367(10) . ? C78 C79 1.373(9) . ? C101 C102 1.373(11) . ? C101 C106 1.365(12) . ? C101 C107 1.504(12) . ? C102 H102 0.9500 . ? C102 C103 1.386(12) . ? C103 H103 0.9500 . ? C103 C104 1.389(12) . ? C104 H104 0.9500 . ? C104 C105 1.387(12) . ? C105 H105 0.9500 . ? C105 C106 1.400(13) . ? C106 H106 0.9500 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? C111 C112 1.380(11) . ? C111 C116 1.394(11) . ? C111 C117 1.511(11) . ? C112 H112 0.9500 . ? C112 C113 1.375(11) . ? C113 H113 0.9500 . ? C113 C114 1.381(12) . ? C114 H114 0.9500 . ? C114 C115 1.382(11) . ? C115 H115 0.9500 . ? C115 C116 1.398(12) . ? C116 H116 0.9500 . ? C117 H11A 0.9800 . ? C117 H11B 0.9800 . ? C117 H11C 0.9800 . ? 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 -0.0072 -35.8462 0.8493 -0.0789 0.9926 -0.0921 0.0072 35.8462 -0.8493 0.0789 -0.9926 0.0921 -0.0236 2.4866 8.7674 0.7919 0.1459 0.5930 0.0236 -2.4866 -8.7674 -0.7919 -0.1459 -0.5930 3.6074 4.8857 -1.2146 -0.5900 -0.1124 0.7995 -3.6074 -4.8857 1.2146 0.5900 0.1124 -0.7995 0.9977 4.0893 7.9997 0.5882 0.0978 0.7918