#------------------------------------------------------------------------------ #$Date: 2024-07-05 18:35:15 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292979 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248666.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_7248666 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 'C14 Ag2 F10 O4, C12 H10 O' _chemical_formula_sum 'C26 H10 Ag2 F10 O5' _chemical_formula_weight 808.08 _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 2023-10-20 _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 103.760(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6080(4) _cell_length_b 9.2325(2) _cell_length_c 18.5937(4) _cell_measurement_reflns_used 8026 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 74.6810 _cell_measurement_theta_min 3.4590 _cell_volume 2435.73(10) _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 1.000 _diffrn_measured_fraction_theta_max 0.999 _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 71.00 96.00 0.50 1.20 -- 102.12 -99.00 -60.00 50 2 \w -8.00 21.00 0.50 0.40 -- -51.89 59.00 93.00 58 3 \w -57.00 -31.00 0.50 1.20 -- -87.58 59.00 93.00 52 4 \w -54.00 -13.00 0.50 1.20 -- -87.58 57.00 30.00 82 5 \w -3.00 23.00 0.50 0.40 -- -51.89 19.00 90.00 52 6 \w -27.00 24.00 0.50 0.40 -- -51.89 38.00-150.00 102 7 \w -3.00 25.00 0.50 0.40 -- -51.89 19.00-180.00 56 8 \w -53.00 -13.00 0.50 1.20 -- -87.58 57.00-180.00 80 9 \w -118.00 -71.00 0.50 1.20 -- -87.58 -59.00 -46.00 94 10 \w -119.00 -89.00 0.50 0.40 -- -51.89 -59.00 -46.00 60 11 \w -148.00-123.00 0.50 1.20 -- -87.58 -59.00 -46.00 50 12 \w -151.00-124.00 0.50 1.20 -- -87.58 -99.00 90.00 54 13 \w -120.00 -88.00 0.50 1.20 -- -87.58 -99.00 90.00 64 14 \w 42.00 68.00 0.50 0.40 -- 51.89 59.00 93.00 52 15 \w 93.00 125.00 0.50 0.40 -- 51.89 59.00 93.00 64 16 \w 116.00 145.00 0.50 1.20 -- 102.12 59.00 93.00 58 17 \w 148.00 174.00 0.50 1.20 -- 102.12 19.00 60.00 52 18 \w 79.00 123.00 0.50 1.20 -- 102.12 19.00 60.00 88 19 \w 67.00 172.00 0.50 1.20 -- 102.12 19.00-120.00 210 20 \w 26.00 51.00 0.50 1.20 -- 102.12 -38.00-150.00 50 21 \w 44.00 79.00 0.50 1.20 -- 102.12 -57.00-180.00 70 22 \w -17.00 57.00 0.50 0.40 -- 51.89 -59.00 -46.00 148 23 \w 29.00 72.00 0.50 1.20 -- 102.12 -57.00 30.00 86 24 \w 40.00 70.00 0.50 1.20 -- 102.12 -57.00 0.00 60 25 \w 29.00 58.00 0.50 1.20 -- 102.12 -59.00 -46.00 58 26 \w 42.00 67.00 0.50 1.20 -- 102.12 -57.00-150.00 50 27 \w 25.00 51.00 0.50 1.20 -- 102.12 -38.00-120.00 52 28 \w 42.00 75.00 0.50 1.20 -- 102.12 -57.00 -90.00 66 29 \w 25.00 50.00 0.50 1.20 -- 102.12 -38.00 -90.00 50 30 \w 36.00 72.00 0.50 1.20 -- 102.12 -57.00 -30.00 72 31 \w 27.00 52.00 0.50 1.20 -- 102.12 -38.00 30.00 50 32 \w 27.00 52.00 0.50 1.20 -- 102.12 -38.00 90.00 50 33 \w 25.00 50.00 0.50 1.20 -- 102.12 -38.00 60.00 50 34 \w 27.00 52.00 0.50 1.20 -- 102.12 -38.00 120.00 50 35 \w 40.00 68.00 0.50 1.20 -- 102.12 -57.00 150.00 56 ; _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 0.0012552000 _diffrn_orient_matrix_UB_12 0.1074898000 _diffrn_orient_matrix_UB_13 -0.0631390000 _diffrn_orient_matrix_UB_21 0.1008515000 _diffrn_orient_matrix_UB_22 0.0461169000 _diffrn_orient_matrix_UB_23 0.0393177000 _diffrn_orient_matrix_UB_31 0.0401943000 _diffrn_orient_matrix_UB_32 -0.1190298000 _diffrn_orient_matrix_UB_33 -0.0417674000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 21580 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.489 _diffrn_reflns_theta_min 3.474 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.999 _exptl_absorpt_correction_T_max 0.84608 _exptl_absorpt_correction_T_min 0.84372 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023) Spherical absorption correction using equivalent radius and absorption coefficient. 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 2.204 _exptl_crystal_description needle _exptl_crystal_F_000 1560 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: diphenyl ether/pentane (at 303 Kelvin)' _exptl_crystal_size_max 0.063 _exptl_crystal_size_mid 0.026 _exptl_crystal_size_min 0.014 _exptl_crystal_size_rad 0.016 _refine_diff_density_max 1.599 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 4976 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0332 _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^)+(0.0345P)^2^+3.6299P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0792 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4086 _reflns_number_total 4976 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_Ph2O _cod_depositor_comments 'Adding full bibliography for 7248652--7248666.cif.' _cod_database_code 7248666 _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 0.828 _shelx_estimated_absorpt_t_min 0.473 _diffrn_oxdiff_digest_frames ; 017f4026392446966c76f3c313c52913e702396d252 ; _diffrn_oxdiff_digest_hkl ; 01dcdef9deecfba09a439d82c6e71b8235ab9a ; _reflns_odcompleteness_completeness 99.91 _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: C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C109(H109), C110(H110), C111(H111), C112(H112), C113(H113) ; _shelx_res_file ; TITL ohd491_2_scale2_a.res in P2(1)/n REM Old TITL OHD491_2_scale2 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.154, Rweak 0.006, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C26 O5 F10 Ag2 CELL 1.54184 14.608 9.2325 18.5937 90 103.76 90 ZERR 4 0.0004 0.0002 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 104 40 8 40 20 EQIV $1 1.5-X,0.5+Y,1.5-Z L.S. 4 0 0 PLAN 20 SIZE 0.014 0.026 0.063 TEMP -153.15 BIND C104 Ag1 BIND Ag2 C109_$1 BIND Ag2 C110_$1 BOND $H list 4 fmap 2 53 ACTA SHEL 50 0.8 REM REM REM WGHT 0.034500 3.629900 FVAR 0.25761 AG1 3 0.708668 0.849137 0.656234 11.00000 0.05736 0.02266 = 0.02333 0.00074 0.01470 0.00386 AG2 3 0.794424 0.574248 0.680466 11.00000 0.05781 0.02265 = 0.02496 0.00441 0.01729 0.00557 F20 4 0.920311 0.912656 0.485134 11.00000 0.04022 0.03337 = 0.03485 -0.00472 0.00911 -0.01305 F21 4 0.939033 0.925591 0.344942 11.00000 0.05195 0.03748 = 0.04524 0.00800 0.02569 -0.00750 F22 4 0.834861 0.748748 0.239971 11.00000 0.06635 0.04182 = 0.02799 0.00150 0.02350 0.00540 F23 4 0.714188 0.555037 0.276809 11.00000 0.06220 0.04391 = 0.02683 -0.01256 0.00695 -0.01128 F24 4 0.697988 0.535750 0.417464 11.00000 0.04501 0.03793 = 0.03347 -0.00581 0.01180 -0.01846 F40 4 0.570176 0.843608 0.854356 11.00000 0.03718 0.03221 = 0.03583 0.00386 0.00519 0.00590 F41 4 0.547372 0.847456 0.992988 11.00000 0.04260 0.04722 = 0.04911 -0.00716 0.02444 0.00473 F42 4 0.672592 0.708888 1.103086 11.00000 0.06067 0.06201 = 0.02647 -0.00428 0.02134 -0.00575 F43 4 0.825034 0.575559 1.074035 11.00000 0.04814 0.04831 = 0.02632 0.00704 0.00200 0.00168 F44 4 0.856892 0.586102 0.938704 11.00000 0.03381 0.02829 = 0.03212 -0.00020 0.00900 0.00537 O11 5 0.776886 0.836576 0.560457 11.00000 0.04200 0.02361 = 0.02487 0.00012 0.01288 0.00206 O13 5 0.806653 0.596650 0.565339 11.00000 0.03699 0.02363 = 0.02632 0.00168 0.00938 -0.00080 O31 5 0.707711 0.827415 0.775884 11.00000 0.05010 0.02061 = 0.02278 0.00159 0.01228 0.00316 O33 5 0.758995 0.597874 0.791123 11.00000 0.05348 0.02035 = 0.02310 -0.00157 0.01377 0.00158 O101 5 0.565437 0.343742 0.643415 11.00000 0.05533 0.03435 = 0.05373 -0.00166 0.03158 0.00005 C12 1 0.796327 0.718400 0.534477 11.00000 0.02456 0.02319 = 0.02547 -0.00256 0.00611 -0.00062 C14 1 0.808472 0.723895 0.455799 11.00000 0.02900 0.02227 = 0.02445 0.00118 0.00687 0.00163 C15 1 0.867217 0.823389 0.434493 11.00000 0.03118 0.02228 = 0.03162 -0.00022 0.00898 -0.00370 C16 1 0.878031 0.831878 0.362992 11.00000 0.03423 0.02620 = 0.03418 0.00492 0.01595 -0.00126 C17 1 0.826289 0.741330 0.309646 11.00000 0.04235 0.02803 = 0.02488 0.00184 0.01435 0.00799 C18 1 0.765584 0.641902 0.328708 11.00000 0.03571 0.03019 = 0.02606 -0.00538 0.00542 0.00174 C19 1 0.758056 0.633346 0.401109 11.00000 0.03204 0.02496 = 0.02834 -0.00016 0.00975 -0.00300 C32 1 0.728596 0.712537 0.813257 11.00000 0.03317 0.02086 = 0.02013 0.00000 0.00769 -0.00221 C34 1 0.714506 0.715045 0.890593 11.00000 0.03772 0.01757 = 0.02274 0.00023 0.00817 -0.00207 C35 1 0.636646 0.779635 0.907798 11.00000 0.03363 0.02378 = 0.02868 0.00086 0.00670 -0.00377 C36 1 0.623018 0.781042 0.978873 11.00000 0.03439 0.02933 = 0.03786 -0.00526 0.01588 -0.00272 C37 1 0.686807 0.712740 1.034695 11.00000 0.04827 0.03444 = 0.02197 -0.00493 0.01389 -0.00867 C38 1 0.764416 0.646678 1.019858 11.00000 0.03967 0.02625 = 0.02293 -0.00026 0.00474 -0.00406 C39 1 0.778457 0.649632 0.949511 11.00000 0.03389 0.02142 = 0.02867 -0.00146 0.00900 -0.00299 C102 1 0.553622 0.490371 0.629098 11.00000 0.03206 0.03446 = 0.03701 -0.00534 0.00998 -0.00612 C103 1 0.588695 0.539841 0.570703 11.00000 0.03542 0.05145 = 0.03609 -0.00312 0.01445 -0.00439 AFIX 43 H103 2 0.621079 0.475274 0.545578 11.00000 -1.20000 AFIX 0 C104 1 0.576726 0.682455 0.548976 11.00000 0.03119 0.05321 = 0.03777 0.00810 0.00639 -0.01057 AFIX 43 H104 2 0.599456 0.715370 0.508029 11.00000 -1.20000 AFIX 0 C105 1 0.531641 0.778474 0.586537 11.00000 0.03625 0.04152 = 0.04836 0.00957 0.00879 -0.00335 AFIX 43 H105 2 0.523422 0.876902 0.571490 11.00000 -1.20000 AFIX 0 C106 1 0.498592 0.729232 0.646436 11.00000 0.03891 0.04024 = 0.04635 0.00321 0.01553 0.00228 AFIX 43 H106 2 0.469505 0.795060 0.673395 11.00000 -1.20000 AFIX 0 C107 1 0.507893 0.584329 0.667038 11.00000 0.03879 0.03768 = 0.03948 0.00046 0.01793 -0.00261 AFIX 43 H107 2 0.483159 0.550005 0.706730 11.00000 -1.20000 AFIX 0 C108 1 0.524641 0.278587 0.695687 11.00000 0.03737 0.02978 = 0.04052 -0.00118 0.01579 0.00243 C109 1 0.550865 0.314955 0.770025 11.00000 0.03447 0.03609 = 0.04280 -0.00469 0.00446 0.00228 AFIX 43 H109 2 0.596446 0.388458 0.786825 11.00000 -1.20000 AFIX 0 C110 1 0.509883 0.242977 0.819274 11.00000 0.04137 0.04268 = 0.03164 -0.00128 0.00220 0.00937 AFIX 43 H110 2 0.526972 0.268079 0.870269 11.00000 -1.20000 AFIX 0 C111 1 0.443948 0.134256 0.795395 11.00000 0.05101 0.03190 = 0.03789 0.00428 0.01633 0.00439 AFIX 43 H111 2 0.416044 0.085084 0.829689 11.00000 -1.20000 AFIX 0 C112 1 0.419260 0.098243 0.720510 11.00000 0.05228 0.02952 = 0.04074 -0.00512 0.01433 -0.00489 AFIX 43 H112 2 0.374465 0.023731 0.703587 11.00000 -1.20000 AFIX 0 C113 1 0.459603 0.170351 0.670838 11.00000 0.04711 0.03085 = 0.03555 -0.00597 0.01138 -0.00012 AFIX 43 H113 2 0.442720 0.145660 0.619785 11.00000 -1.20000 AFIX 0 HKLF 4 REM ohd491_2_scale2_a.res in P2(1)/n REM R1 = 0.0332 for 4086 Fo > 4sig(Fo) and 0.0444 for all 4976 data REM 388 parameters refined using 0 restraints END WGHT 0.0345 3.6299 REM Highest difference peak 1.599, deepest hole -1.070, 1-sigma level 0.097 Q1 1 0.7741 0.8589 0.6758 11.00000 0.05 1.60 Q2 1 0.7156 0.9367 0.8181 11.00000 0.05 0.62 Q3 1 0.7069 0.9873 0.6564 11.00000 0.05 0.58 Q4 1 0.7309 0.7179 0.6642 11.00000 0.05 0.58 Q5 1 0.7289 0.5673 0.6614 11.00000 0.05 0.50 Q6 1 0.8107 0.7142 0.6821 11.00000 0.05 0.50 Q7 1 0.6980 0.8336 0.6985 11.00000 0.05 0.42 Q8 1 0.8076 0.7217 0.4955 11.00000 0.05 0.40 Q9 1 0.8803 0.8203 0.3997 11.00000 0.05 0.40 Q10 1 0.6844 0.8185 0.5786 11.00000 0.05 0.40 Q11 1 0.7642 0.8407 0.5992 11.00000 0.05 0.39 Q12 1 0.8021 0.6567 0.6128 11.00000 0.05 0.38 Q13 1 0.6417 0.8379 0.6964 11.00000 0.05 0.38 Q14 1 0.7223 0.5824 0.7201 11.00000 0.05 0.38 Q15 1 0.7667 0.5842 0.7452 11.00000 0.05 0.36 Q16 1 0.7818 0.8279 0.6127 11.00000 0.05 0.36 Q17 1 0.7483 0.6535 0.6206 11.00000 0.05 0.36 Q18 1 0.7327 0.7493 0.5999 11.00000 0.05 0.35 Q19 1 0.6864 0.9294 0.7120 11.00000 0.05 0.35 Q20 1 0.7995 0.5671 0.6221 11.00000 0.05 0.34 ; _shelx_res_checksum 96346 _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 1.227 _oxdiff_exptl_absorpt_empirical_full_min 0.839 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 0.70867(2) 0.84914(3) 0.65623(2) 0.03359(9) Uani 1 1 d . . . . . Ag2 Ag 0.79442(2) 0.57425(3) 0.68047(2) 0.03389(9) Uani 1 1 d . . . . . F20 F 0.92031(17) 0.9127(3) 0.48513(13) 0.0361(5) Uani 1 1 d . . . . . F21 F 0.93903(18) 0.9256(3) 0.34494(14) 0.0425(6) Uani 1 1 d . . . . . F22 F 0.83486(19) 0.7487(3) 0.23997(12) 0.0433(6) Uani 1 1 d . . . . . F23 F 0.71419(19) 0.5550(3) 0.27681(13) 0.0449(6) Uani 1 1 d . . . . . F24 F 0.69799(17) 0.5358(3) 0.41746(12) 0.0384(6) Uani 1 1 d . . . . . F40 F 0.57018(16) 0.8436(3) 0.85436(13) 0.0357(5) Uani 1 1 d . . . . . F41 F 0.54737(18) 0.8475(3) 0.99299(14) 0.0440(6) Uani 1 1 d . . . . . F42 F 0.67259(19) 0.7089(3) 1.10309(13) 0.0479(7) Uani 1 1 d . . . . . F43 F 0.82503(18) 0.5756(3) 1.07403(12) 0.0421(6) Uani 1 1 d . . . . . F44 F 0.85689(15) 0.5861(2) 0.93870(12) 0.0312(5) Uani 1 1 d . . . . . O11 O 0.7769(2) 0.8366(3) 0.56046(14) 0.0293(6) Uani 1 1 d . . . . . O13 O 0.80665(19) 0.5966(3) 0.56534(14) 0.0287(6) Uani 1 1 d . . . . . O31 O 0.7077(2) 0.8274(3) 0.77588(14) 0.0306(6) Uani 1 1 d . . . . . O33 O 0.7590(2) 0.5979(3) 0.79112(14) 0.0315(6) Uani 1 1 d . . . . . O101 O 0.5654(2) 0.3437(3) 0.64341(18) 0.0447(8) Uani 1 1 d . . . . . C12 C 0.7963(2) 0.7184(4) 0.53448(19) 0.0244(7) Uani 1 1 d . . . . . C14 C 0.8085(3) 0.7239(4) 0.4558(2) 0.0252(7) Uani 1 1 d . . . . . C15 C 0.8672(3) 0.8234(4) 0.4345(2) 0.0281(8) Uani 1 1 d . . . . . C16 C 0.8780(3) 0.8319(4) 0.3630(2) 0.0302(8) Uani 1 1 d . . . . . C17 C 0.8263(3) 0.7413(4) 0.3096(2) 0.0307(8) Uani 1 1 d . . . . . C18 C 0.7656(3) 0.6419(4) 0.3287(2) 0.0310(8) Uani 1 1 d . . . . . C19 C 0.7581(3) 0.6333(4) 0.4011(2) 0.0280(8) Uani 1 1 d . . . . . C32 C 0.7286(3) 0.7125(4) 0.81326(19) 0.0245(7) Uani 1 1 d . . . . . C34 C 0.7145(3) 0.7150(4) 0.89059(19) 0.0258(8) Uani 1 1 d . . . . . C35 C 0.6366(3) 0.7796(4) 0.9078(2) 0.0288(8) Uani 1 1 d . . . . . C36 C 0.6230(3) 0.7810(5) 0.9789(2) 0.0326(9) Uani 1 1 d . . . . . C37 C 0.6868(3) 0.7127(5) 1.0347(2) 0.0340(9) Uani 1 1 d . . . . . C38 C 0.7644(3) 0.6467(4) 1.0199(2) 0.0301(8) Uani 1 1 d . . . . . C39 C 0.7785(3) 0.6496(4) 0.9495(2) 0.0277(8) Uani 1 1 d . . . . . C102 C 0.5536(3) 0.4904(5) 0.6291(2) 0.0342(9) Uani 1 1 d . . . . . C103 C 0.5887(3) 0.5398(5) 0.5707(2) 0.0400(10) Uani 1 1 d . . . . . H103 H 0.6211 0.4753 0.5456 0.048 Uiso 1 1 calc R . . . . C104 C 0.5767(3) 0.6825(5) 0.5490(2) 0.0410(11) Uani 1 1 d . . . . . H104 H 0.5995 0.7154 0.5080 0.049 Uiso 1 1 calc R . . . . C105 C 0.5316(3) 0.7785(5) 0.5865(3) 0.0423(10) Uani 1 1 d . . . . . H105 H 0.5234 0.8769 0.5715 0.051 Uiso 1 1 calc R . . . . C106 C 0.4986(3) 0.7292(5) 0.6464(3) 0.0409(10) Uani 1 1 d . . . . . H106 H 0.4695 0.7951 0.6734 0.049 Uiso 1 1 calc R . . . . C107 C 0.5079(3) 0.5843(5) 0.6670(2) 0.0372(9) Uani 1 1 d . . . . . H107 H 0.4832 0.5500 0.7067 0.045 Uiso 1 1 calc R . . . . C108 C 0.5246(3) 0.2786(5) 0.6957(2) 0.0348(9) Uani 1 1 d . . . . . C109 C 0.5509(3) 0.3150(5) 0.7700(2) 0.0386(10) Uani 1 1 d . . . . . H109 H 0.5964 0.3885 0.7868 0.046 Uiso 1 1 calc R . . . . C110 C 0.5099(3) 0.2430(5) 0.8193(2) 0.0397(10) Uani 1 1 d . . . . . H110 H 0.5270 0.2681 0.8703 0.048 Uiso 1 1 calc R . . . . C111 C 0.4439(3) 0.1343(5) 0.7954(2) 0.0393(10) Uani 1 1 d . . . . . H111 H 0.4160 0.0851 0.8297 0.047 Uiso 1 1 calc R . . . . C112 C 0.4193(3) 0.0982(5) 0.7205(2) 0.0403(10) Uani 1 1 d . . . . . H112 H 0.3745 0.0237 0.7036 0.048 Uiso 1 1 calc R . . . . C113 C 0.4596(3) 0.1704(5) 0.6708(2) 0.0376(10) Uani 1 1 d . . . . . H113 H 0.4427 0.1457 0.6198 0.045 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 0.0574(2) 0.02266(15) 0.02333(14) 0.00074(11) 0.01470(12) 0.00386(13) Ag2 0.0578(2) 0.02265(15) 0.02496(14) 0.00441(11) 0.01729(12) 0.00557(13) F20 0.0402(13) 0.0334(13) 0.0348(12) -0.0047(10) 0.0091(10) -0.0130(10) F21 0.0519(15) 0.0375(14) 0.0452(14) 0.0080(11) 0.0257(12) -0.0075(12) F22 0.0664(17) 0.0418(14) 0.0280(12) 0.0015(11) 0.0235(11) 0.0054(13) F23 0.0622(16) 0.0439(15) 0.0268(11) -0.0126(11) 0.0069(11) -0.0113(13) F24 0.0450(14) 0.0379(14) 0.0335(12) -0.0058(10) 0.0118(10) -0.0185(11) F40 0.0372(12) 0.0322(13) 0.0358(12) 0.0039(10) 0.0052(10) 0.0059(10) F41 0.0426(14) 0.0472(16) 0.0491(15) -0.0072(12) 0.0244(12) 0.0047(12) F42 0.0607(16) 0.0620(18) 0.0265(11) -0.0043(12) 0.0213(11) -0.0058(14) F43 0.0481(14) 0.0483(16) 0.0263(11) 0.0070(11) 0.0020(10) 0.0017(12) F44 0.0338(12) 0.0283(12) 0.0321(11) -0.0002(9) 0.0090(9) 0.0054(9) O11 0.0420(15) 0.0236(14) 0.0249(13) 0.0001(11) 0.0129(11) 0.0021(12) O13 0.0370(15) 0.0236(14) 0.0263(13) 0.0017(11) 0.0094(11) -0.0008(11) O31 0.0501(17) 0.0206(13) 0.0228(12) 0.0016(11) 0.0123(12) 0.0032(12) O33 0.0535(17) 0.0203(13) 0.0231(12) -0.0016(11) 0.0138(12) 0.0016(12) O101 0.0553(19) 0.0344(17) 0.0537(19) -0.0017(15) 0.0316(16) 0.0001(15) C12 0.0246(17) 0.0232(18) 0.0255(18) -0.0026(15) 0.0061(14) -0.0006(15) C14 0.0290(18) 0.0223(18) 0.0244(17) 0.0012(15) 0.0069(14) 0.0016(15) C15 0.031(2) 0.0223(19) 0.0316(19) -0.0002(15) 0.0090(16) -0.0037(15) C16 0.034(2) 0.026(2) 0.034(2) 0.0049(17) 0.0159(16) -0.0013(16) C17 0.042(2) 0.028(2) 0.0249(18) 0.0018(16) 0.0143(16) 0.0080(17) C18 0.036(2) 0.030(2) 0.0261(18) -0.0054(16) 0.0054(16) 0.0017(17) C19 0.0320(19) 0.0250(19) 0.0283(18) -0.0002(16) 0.0098(15) -0.0030(16) C32 0.0332(19) 0.0209(18) 0.0201(16) 0.0000(15) 0.0077(14) -0.0022(15) C34 0.038(2) 0.0176(17) 0.0227(17) 0.0002(14) 0.0082(15) -0.0021(15) C35 0.034(2) 0.0238(19) 0.0287(18) 0.0009(16) 0.0067(15) -0.0038(16) C36 0.034(2) 0.029(2) 0.038(2) -0.0053(18) 0.0159(17) -0.0027(17) C37 0.048(2) 0.034(2) 0.0220(18) -0.0049(17) 0.0139(17) -0.0087(19) C38 0.040(2) 0.026(2) 0.0229(17) -0.0003(16) 0.0047(16) -0.0041(17) C39 0.034(2) 0.0214(18) 0.0287(18) -0.0015(15) 0.0090(15) -0.0030(16) C102 0.032(2) 0.034(2) 0.037(2) -0.0053(18) 0.0100(17) -0.0061(18) C103 0.035(2) 0.051(3) 0.036(2) -0.003(2) 0.0144(18) -0.004(2) C104 0.031(2) 0.053(3) 0.038(2) 0.008(2) 0.0064(18) -0.011(2) C105 0.036(2) 0.042(3) 0.048(3) 0.010(2) 0.0088(19) -0.003(2) C106 0.039(2) 0.040(3) 0.046(2) 0.003(2) 0.0155(19) 0.002(2) C107 0.039(2) 0.038(2) 0.039(2) 0.0005(19) 0.0179(18) -0.0026(19) C108 0.037(2) 0.030(2) 0.041(2) -0.0012(18) 0.0158(18) 0.0024(18) C109 0.034(2) 0.036(2) 0.043(2) -0.0047(19) 0.0045(18) 0.0023(18) C110 0.041(2) 0.043(3) 0.032(2) -0.0013(19) 0.0022(18) 0.009(2) C111 0.051(3) 0.032(2) 0.038(2) 0.0043(19) 0.016(2) 0.004(2) C112 0.052(3) 0.030(2) 0.041(2) -0.0051(19) 0.014(2) -0.0049(19) C113 0.047(2) 0.031(2) 0.036(2) -0.0060(18) 0.0114(19) -0.0001(19) 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 7 0 -10 0.0072 -7 0 10 0.0072 7 2 6 0.0120 -7 -2 -6 0.0120 1 6 -1 0.0276 -1 -6 1 0.0276 9 0 -3 0.0082 3 2 -11 0.0139 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 Ag2 Ag1 C104 80.08(10) . . ? O11 Ag1 Ag2 79.38(7) . . ? O11 Ag1 O33 106.30(9) . 2_656 ? O11 Ag1 C104 76.82(11) . . ? O11 Ag1 C105 99.40(13) . . ? O31 Ag1 Ag2 82.41(7) . . ? O31 Ag1 O11 153.48(10) . . ? O31 Ag1 O33 74.81(9) . 2_656 ? O31 Ag1 C104 118.76(12) . . ? O31 Ag1 C105 103.02(13) . . ? O33 Ag1 Ag2 136.88(7) 2_656 . ? O33 Ag1 C104 143.03(12) 2_656 . ? O33 Ag1 C105 118.93(13) 2_656 . ? C105 Ag1 Ag2 101.48(11) . . ? C105 Ag1 C104 28.70(14) . . ? Ag1 Ag2 C109 70.85(8) . 2_656 ? Ag1 Ag2 C110 85.76(9) . 2_656 ? O13 Ag2 Ag1 84.01(7) . . ? O13 Ag2 O31 115.16(9) . 2_646 ? O13 Ag2 O33 166.17(10) . . ? O13 Ag2 C109 89.96(11) . 2_656 ? O13 Ag2 C110 71.45(10) . 2_656 ? O31 Ag2 Ag1 149.34(7) 2_646 . ? O31 Ag2 C109 129.20(11) 2_646 2_656 ? O31 Ag2 C110 122.09(11) 2_646 2_656 ? O33 Ag2 Ag1 82.45(7) . . ? O33 Ag2 O31 76.14(9) . 2_646 ? O33 Ag2 C109 88.25(11) . 2_656 ? O33 Ag2 C110 110.21(11) . 2_656 ? C109 Ag2 C110 24.79(12) 2_656 2_656 ? C12 O11 Ag1 122.4(2) . . ? C12 O13 Ag2 120.0(2) . . ? Ag1 O31 Ag2 104.63(10) . 2_656 ? C32 O31 Ag1 124.3(2) . . ? C32 O31 Ag2 128.7(2) . 2_656 ? Ag2 O33 Ag1 101.90(10) . 2_646 ? C32 O33 Ag1 134.1(2) . 2_646 ? C32 O33 Ag2 124.0(2) . . ? C102 O101 C108 120.2(3) . . ? O11 C12 O13 128.1(3) . . ? O11 C12 C14 115.6(3) . . ? O13 C12 C14 116.3(3) . . ? C15 C14 C12 121.6(3) . . ? C15 C14 C19 116.7(3) . . ? C19 C14 C12 121.6(3) . . ? F20 C15 C14 120.0(3) . . ? F20 C15 C16 117.4(3) . . ? C16 C15 C14 122.5(4) . . ? F21 C16 C15 120.9(4) . . ? F21 C16 C17 119.7(3) . . ? C17 C16 C15 119.4(4) . . ? F22 C17 C16 120.4(4) . . ? F22 C17 C18 119.9(4) . . ? C16 C17 C18 119.7(3) . . ? F23 C18 C17 119.8(3) . . ? F23 C18 C19 120.5(4) . . ? C19 C18 C17 119.6(4) . . ? F24 C19 C14 120.1(3) . . ? F24 C19 C18 117.9(3) . . ? C18 C19 C14 122.0(4) . . ? O31 C32 C34 116.3(3) . . ? O33 C32 O31 125.8(3) . . ? O33 C32 C34 117.9(3) . . ? C35 C34 C32 122.3(3) . . ? C35 C34 C39 115.9(3) . . ? C39 C34 C32 121.8(3) . . ? F40 C35 C34 120.3(3) . . ? F40 C35 C36 117.3(3) . . ? C36 C35 C34 122.5(4) . . ? F41 C36 C35 120.2(4) . . ? F41 C36 C37 120.3(4) . . ? C37 C36 C35 119.5(4) . . ? F42 C37 C36 120.0(4) . . ? F42 C37 C38 120.1(4) . . ? C38 C37 C36 119.8(4) . . ? F43 C38 C37 119.7(3) . . ? F43 C38 C39 120.2(4) . . ? C39 C38 C37 120.1(4) . . ? F44 C39 C34 120.4(3) . . ? F44 C39 C38 117.4(3) . . ? C38 C39 C34 122.2(4) . . ? O101 C102 C103 114.9(4) . . ? O101 C102 C107 124.6(4) . . ? C103 C102 C107 120.4(4) . . ? C102 C103 H103 120.0 . . ? C104 C103 C102 120.1(4) . . ? C104 C103 H103 120.0 . . ? Ag1 C104 H104 94.6 . . ? C103 C104 Ag1 107.0(3) . . ? C103 C104 H104 119.8 . . ? C103 C104 C105 120.4(4) . . ? C105 C104 Ag1 68.2(3) . . ? C105 C104 H104 119.8 . . ? Ag1 C105 H105 87.1 . . ? C104 C105 Ag1 83.1(3) . . ? C104 C105 H105 120.3 . . ? C104 C105 C106 119.4(4) . . ? C106 C105 Ag1 99.8(3) . . ? C106 C105 H105 120.3 . . ? C105 C106 H106 119.8 . . ? C107 C106 C105 120.4(4) . . ? C107 C106 H106 119.8 . . ? C102 C107 C106 119.3(4) . . ? C102 C107 H107 120.3 . . ? C106 C107 H107 120.3 . . ? C109 C108 O101 122.0(4) . . ? C113 C108 O101 117.0(4) . . ? C113 C108 C109 121.0(4) . . ? C108 C109 H109 120.5 . . ? C110 C109 C108 119.0(4) . . ? C110 C109 H109 120.5 . . ? C109 C110 H110 119.5 . . ? C109 C110 C111 120.9(4) . . ? C111 C110 H110 119.5 . . ? C110 C111 H111 120.4 . . ? C110 C111 C112 119.1(4) . . ? C112 C111 H111 120.4 . . ? C111 C112 H112 119.9 . . ? C113 C112 C111 120.3(4) . . ? C113 C112 H112 119.9 . . ? C108 C113 H113 120.2 . . ? C112 C113 C108 119.7(4) . . ? C112 C113 H113 120.2 . . ? 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 2.8187(4) . ? Ag1 O11 2.241(3) . ? Ag1 O31 2.237(3) . ? Ag1 O33 2.497(3) 2_656 ? Ag1 C104 2.869(4) . ? Ag1 C105 2.683(4) . ? Ag2 O13 2.200(3) . ? Ag2 O31 2.422(3) 2_646 ? Ag2 O33 2.248(3) . ? Ag2 C109 3.147(4) 2_656 ? Ag2 C110 3.255(4) 2_656 ? F20 C15 1.349(4) . ? F21 C16 1.341(4) . ? F22 C17 1.333(4) . ? F23 C18 1.339(4) . ? F24 C19 1.342(4) . ? F40 C35 1.349(4) . ? F41 C36 1.343(5) . ? F42 C37 1.337(4) . ? F43 C38 1.344(4) . ? F44 C39 1.344(4) . ? O11 C12 1.253(4) . ? O13 C12 1.255(4) . ? O31 Ag2 2.422(3) 2_656 ? O31 C32 1.265(4) . ? O33 Ag1 2.497(3) 2_646 ? O33 C32 1.255(4) . ? O101 C102 1.383(5) . ? O101 C108 1.392(5) . ? C12 C14 1.516(5) . ? C14 C15 1.378(5) . ? C14 C19 1.385(5) . ? C15 C16 1.378(5) . ? C16 C17 1.377(6) . ? C17 C18 1.380(6) . ? C18 C19 1.379(5) . ? C32 C34 1.500(5) . ? C34 C35 1.387(5) . ? C34 C39 1.397(5) . ? C35 C36 1.383(5) . ? C36 C37 1.372(6) . ? C37 C38 1.372(6) . ? C38 C39 1.372(5) . ? C102 C103 1.384(6) . ? C102 C107 1.386(6) . ? C103 H103 0.9500 . ? C103 C104 1.376(7) . ? C104 H104 0.9500 . ? C104 C105 1.388(7) . ? C105 H105 0.9500 . ? C105 C106 1.391(6) . ? C106 H106 0.9500 . ? C106 C107 1.389(6) . ? C107 H107 0.9500 . ? C108 C109 1.385(6) . ? C108 C113 1.381(6) . ? C109 H109 0.9500 . ? C109 C110 1.378(7) . ? C110 H110 0.9500 . ? C110 C111 1.389(7) . ? C111 H111 0.9500 . ? C111 C112 1.393(6) . ? C112 H112 0.9500 . ? C112 C113 1.379(6) . ? C113 H113 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 7.2229 -0.0142 -9.7873 0.6255 0.3430 0.7008 -7.2229 0.0142 9.7873 -0.6255 -0.3430 -0.7008 6.7263 1.5547 5.6436 -0.1808 0.9720 -0.1504 -6.7263 -1.5547 -5.6436 0.1808 -0.9720 0.1504 0.5157 5.9694 -0.9544 0.7026 0.2898 -0.6500 -0.5157 -5.9694 0.9544 -0.7026 -0.2898 0.6500 9.4697 -0.2465 -3.2850 0.1928 0.8145 0.5472 3.0018 1.9988 -10.9890 0.9125 -0.0372 0.3417