#------------------------------------------------------------------------------ #$Date: 2024-07-05 18:35:15 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292979 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248664.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_7248664 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 'C12 H10 Ag F5 O3' _chemical_formula_sum 'C12 H10 Ag F5 O3' _chemical_formula_weight 405.07 _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 2023-10-27 _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 75.275(3) _cell_angle_beta 85.880(2) _cell_angle_gamma 79.845(3) _cell_formula_units_Z 2 _cell_length_a 5.51822(13) _cell_length_b 9.8945(5) _cell_length_c 13.0489(3) _cell_measurement_reflns_used 10046 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 76.7070 _cell_measurement_theta_min 3.4910 _cell_volume 678.00(4) _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_temperature 120.0 _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 0.994 _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 -116.00 -21.00 0.50 0.10 -- -41.67 140.00 118.00 190 2 \w -121.00 -72.00 0.50 0.10 -- -41.67-130.00-126.00 98 3 \w -110.00 -16.00 0.50 0.10 -- -41.67 130.00 -55.00 188 4 \w -120.00 -65.00 0.50 0.10 -- -41.67-140.00 59.00 110 5 \w 22.00 111.00 0.50 0.10 -- 42.36-130.00-126.00 178 6 \w 71.00 121.00 0.50 0.10 -- 42.36 140.00 118.00 100 7 \w 28.00 117.00 0.50 0.10 -- 42.36-140.00 59.00 178 8 \w -122.00 -21.00 0.50 0.60 -- -89.36 140.00 118.00 202 9 \w -115.00 -16.00 0.50 0.60 -- -89.36 130.00 -55.00 198 10 \w -170.00 -71.00 0.50 0.60 -- -89.36-130.00-126.00 198 11 \w 70.00 173.00 0.50 0.60 -- 113.01 140.00 118.00 206 12 \w 32.00 116.00 0.50 0.60 -- 113.01-130.00-126.00 168 13 \w 77.00 176.00 0.50 0.60 -- 113.01 130.00 -55.00 198 14 \w 34.00 123.00 0.50 0.60 -- 113.01-140.00 59.00 178 15 \w -4.00 45.00 0.50 0.10 -- -41.67 19.00 -30.00 98 16 \w -27.00 45.00 0.50 0.10 -- -41.67 38.00 -30.00 144 17 \w 12.00 124.00 0.50 0.10 -- 42.36 57.00-180.00 224 18 \w 2.00 28.00 0.50 0.10 -- 50.00 96.00 -36.57 52 19 \w 7.00 34.00 0.50 0.10 -- 54.00 94.00 125.28 54 20 \w -153.00 -42.00 0.50 0.10 -- -78.00 -74.00-109.69 222 21 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00 -30.00 64 22 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00-180.00 64 23 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00-150.00 64 24 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00 -60.00 64 25 \w -127.00 -16.00 0.50 0.60 -- -89.36 77.00 150.00 222 26 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00 120.00 64 27 \w -37.00 -5.00 0.50 0.60 -- -89.36 45.00 90.00 64 28 \w -174.00 -69.00 0.50 0.60 -- -95.50 -45.00 98.07 210 29 \w 33.00 111.00 0.50 0.60 -- 113.01-125.00 150.00 156 30 \w 33.00 111.00 0.50 0.60 -- 113.01-125.00 -90.00 156 31 \w 33.00 86.00 0.50 0.60 -- 113.01 -61.00-120.00 106 32 \w 67.00 176.00 0.50 0.60 -- 113.01 30.00 0.00 218 33 \w 33.00 86.00 0.50 0.60 -- 113.01 -61.00 0.00 106 34 \w 28.00 62.00 0.50 0.60 -- 113.01 -45.00 0.00 68 35 \w 80.00 176.00 0.50 0.60 -- 113.01 125.00 30.00 192 36 \w 80.00 176.00 0.50 0.60 -- 113.01 125.00-180.00 192 37 \w 33.00 86.00 0.50 0.60 -- 113.01 -61.00 -90.00 106 38 \w 87.00 176.00 0.50 0.60 -- 113.01 45.00 -60.00 178 39 \w 33.00 111.00 0.50 0.60 -- 113.01-125.00 -30.00 156 40 \w 28.00 62.00 0.50 0.60 -- 113.01 -45.00-180.00 68 41 \w 32.00 105.00 0.50 0.60 -- 113.01 -95.00 150.00 146 42 \w 28.00 62.00 0.50 0.60 -- 113.01 -45.00 120.00 68 43 \w 33.00 86.00 0.50 0.60 -- 113.01 -61.00 120.00 106 44 \w 28.00 62.00 0.50 0.60 -- 113.01 -45.00 -90.00 68 45 \w 28.00 62.00 0.50 0.60 -- 113.01 -45.00-150.00 68 46 \w 87.00 176.00 0.50 0.60 -- 113.01 45.00 30.00 178 47 \w 32.00 105.00 0.50 0.60 -- 113.01 -95.00 0.00 146 48 \w 33.00 86.00 0.50 0.60 -- 113.01 -61.00 60.00 106 49 \w 12.00 124.00 0.50 0.10 -- 42.36 57.00 0.00 224 50 \w 14.00 125.00 0.50 0.10 -- 50.00 75.00 -92.95 222 51 \w 5.00 41.00 0.50 0.10 -- 50.00 91.00 80.92 72 52 \w 9.00 41.00 0.50 0.10 -- 54.00 91.00 179.38 64 53 \w 7.00 34.00 0.50 0.10 -- 54.00 94.00-133.81 54 54 \w 14.00 42.00 0.50 0.10 -- 58.00 88.00 -8.06 56 55 \w 13.00 41.00 0.50 0.10 -- 58.00 91.00 33.57 56 56 \w -145.00 -34.00 0.50 0.10 -- -66.00 -65.00 72.85 222 57 \w -163.00 -52.00 0.50 0.60 -- -89.36 -77.00 0.00 222 58 \w -163.00 -52.00 0.50 0.60 -- -89.36 -77.00 60.00 222 59 \w -171.00 -61.00 0.50 0.60 -- -95.50 -72.00 176.28 220 60 \w 76.00 176.00 0.50 0.60 -- 113.01 77.00 90.00 200 61 \w 67.00 176.00 0.50 0.60 -- 113.01 30.00 -90.00 218 ; _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 0.2829411000 _diffrn_orient_matrix_UB_12 -0.0375901000 _diffrn_orient_matrix_UB_13 0.0023390000 _diffrn_orient_matrix_UB_21 -0.0128771000 _diffrn_orient_matrix_UB_22 -0.0338407000 _diffrn_orient_matrix_UB_23 0.1220171000 _diffrn_orient_matrix_UB_31 -0.0168469000 _diffrn_orient_matrix_UB_32 -0.1551557000 _diffrn_orient_matrix_UB_33 0.0044174000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_unetI/netI 0.0255 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16388 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.497 _diffrn_reflns_theta_min 3.504 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 12.592 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_correction_T_min 0.270 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 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 1.984 _exptl_crystal_description needle _exptl_crystal_F_000 396 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: 2-methyltetrahydrofuran (racemic)/pentane' _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.021 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.982 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 241 _refine_ls_number_reflns 2742 _refine_ls_number_restraints 132 _refine_ls_restrained_S_all 1.114 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0373 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.3722P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.1058 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2470 _reflns_number_total 2742 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_2-MeTHF _cod_depositor_comments 'Adding full bibliography for 7248652--7248666.cif.' _cod_database_code 7248664 _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 0.834 _shelx_estimated_absorpt_t_min 0.235 _diffrn_oxdiff_digest_frames ; 016cb5cba3d5a12b367a4ffdb9688d9c7a08640a26e ; _diffrn_oxdiff_digest_hkl ; 014a30f6f1b72cbf6410635d038f75c62a69bf ; _reflns_odcompleteness_completeness 99.38 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C113-C114 = C104-C103 = C115-C114 1.52 with sigma of 0.02 C104-C105 = C112-C113 1.52 with sigma of 0.01 C102-C103 1.52 with sigma of 0.01 C112-C116 = C102-C106 1.52 with sigma of 0.02 O101-C105 = O111-C115 = O111-C112 = O101-C102 1.44 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O101 \\sim O111 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C103) = Uanis(C102) 4. Others Sof(O111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H11A)=Sof(H11B)=Sof(C114)= Sof(H11C)=Sof(H11D)=Sof(C115)=Sof(H11E)=Sof(H11F)=Sof(C116)=Sof(H11G)= Sof(H11H)=Sof(H11I)=1-FVAR(1) Sof(O101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H10A)=Sof(H10B)=Sof(C104)= Sof(H10C)=Sof(H10D)=Sof(C105)=Sof(H10E)=Sof(H10F)=Sof(C106)=Sof(H10G)= Sof(H10H)=Sof(H10I)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C102(H102), C112(H112) 5.b Secondary CH2 refined with riding coordinates: C103(H10A,H10B), C104(H10C,H10D), C105(H10E,H10F), C113(H11A,H11B), C114(H11C, H11D), C115(H11E,H11F) 5.c Idealised Me refined as rotating group: C106(H10G,H10H,H10I), C116(H11G,H11H,H11I) ; _shelx_res_file ; TITL ohd492_5_numabs_a.res in P-1 REM Old TITL OHD492_5_numabs in P-1 REM SHELXT solution in P-1 REM R1 0.276, Rweak 0.012, Alpha 0.060, Orientation as input REM Formula found by SHELXT: C12 O2 F5 Ag CELL 1.54184 5.518221 9.894488 13.048875 75.2747 85.88 79.8452 ZERR 2 0.000133 0.000462 0.000281 0.0031 0.002 0.0029 LATT 1 SFAC C H Ag F O UNIT 24 20 2 10 6 DFIX 1.52 C113 C114 C104 C103 C115 C114 DFIX 1.52 0.01 C104 C105 C112 C113 DFIX 1.52 0.01 C102 C103 DFIX 1.52 C112 C116 C102 C106 DFIX 1.44 O101 C105 O111 C115 O111 C112 O101 C102 SIMU 0.02 0.04 1.7 O101 O111 C103 > C116 EADP C103 C102 L.S. 4 0 0 PLAN 20 SIZE 0.015 0.021 0.162 TEMP -153.15 BOND $H list 4 fmap 2 53 acta SHEL 50 0.8 REM REM REM WGHT 0.068700 0.372200 FVAR 0.85543 0.63973 AG1 3 -0.202878 0.512370 0.933587 11.00000 0.02634 0.09426 = 0.04199 -0.00764 0.00500 -0.01578 F20 4 0.247932 0.594494 0.613671 11.00000 0.09656 0.16193 = 0.05293 -0.03186 0.01116 -0.08192 F21 4 0.535531 0.712398 0.453399 11.00000 0.13734 0.20333 = 0.04223 -0.03352 0.02727 -0.09078 F22 4 0.817050 0.897633 0.479137 11.00000 0.08682 0.13341 = 0.06462 0.01238 0.02258 -0.05401 F23 4 0.811037 0.965057 0.668458 11.00000 0.10654 0.09600 = 0.09931 -0.00951 0.01071 -0.06238 F24 4 0.532011 0.843616 0.830368 11.00000 0.08220 0.08254 = 0.06371 -0.02467 0.00663 -0.02632 O11 5 0.014039 0.645659 0.810676 11.00000 0.02619 0.10438 = 0.04448 0.00274 -0.00176 -0.01509 O13 5 0.359141 0.574327 0.902819 11.00000 0.02573 0.09127 = 0.03805 0.00195 0.00286 -0.01124 PART 1 O101 5 -0.036626 0.285781 0.897068 21.00000 0.12392 0.12732 = 0.06446 -0.04029 -0.03402 0.04561 PART 0 PART 2 O111 5 -0.135998 0.307530 0.862056 -21.00000 0.13065 0.13176 = 0.10457 -0.05635 0.01354 0.00423 PART 0 C12 1 0.239592 0.638322 0.822376 11.00000 0.02549 0.07353 = 0.03760 -0.00834 0.00460 -0.00946 C14 1 0.382234 0.714360 0.728412 11.00000 0.02733 0.07075 = 0.03889 -0.00232 0.00204 -0.00986 C15 1 0.385199 0.685392 0.630254 11.00000 0.05048 0.09898 = 0.04300 -0.00901 0.00314 -0.03245 C16 1 0.531023 0.747519 0.546918 11.00000 0.06722 0.11810 = 0.03893 -0.00834 0.00938 -0.03559 C17 1 0.674918 0.839030 0.560430 11.00000 0.04996 0.09385 = 0.05106 0.00728 0.00917 -0.02332 C18 1 0.670933 0.873056 0.654786 11.00000 0.04782 0.06892 = 0.06871 0.00304 0.00090 -0.01930 C19 1 0.526451 0.809419 0.738090 11.00000 0.04197 0.06568 = 0.04750 -0.00615 0.00037 -0.00869 PART 1 C102 1 -0.057507 0.236847 0.807024 21.00000 0.14199 0.13345 = 0.09964 -0.05558 0.00663 -0.00728 AFIX 13 H102 2 -0.184488 0.173248 0.826352 21.00000 -1.20000 AFIX 0 C103 1 0.172655 0.145208 0.790628 21.00000 0.14199 0.13345 = 0.09964 -0.05558 0.00663 -0.00728 AFIX 23 H10A 2 0.285871 0.198402 0.740283 21.00000 -1.20000 H10B 2 0.142406 0.064366 0.764345 21.00000 -1.20000 AFIX 0 C104 1 0.273528 0.096019 0.902027 21.00000 0.14517 0.11208 = 0.09859 -0.03687 -0.02128 0.02077 AFIX 23 H10C 2 0.238226 -0.000236 0.936043 21.00000 -1.20000 H10D 2 0.454255 0.092550 0.898660 21.00000 -1.20000 AFIX 0 C105 1 0.154953 0.196797 0.964861 21.00000 0.13498 0.11425 = 0.08129 -0.03791 -0.03808 0.04824 AFIX 23 H10E 2 0.084819 0.146326 1.032864 21.00000 -1.20000 H10F 2 0.273990 0.253086 0.979584 21.00000 -1.20000 AFIX 0 C106 1 -0.169322 0.361990 0.718827 21.00000 0.09726 0.12204 = 0.07993 -0.04697 -0.03937 0.00360 AFIX 137 H10G 2 -0.142665 0.450763 0.733090 21.00000 -1.50000 H10H 2 -0.346458 0.362165 0.716354 21.00000 -1.50000 H10I 2 -0.090378 0.353101 0.650612 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C112 1 0.060649 0.303137 0.781576 -21.00000 0.07253 0.09712 = 0.05528 -0.03604 0.01485 -0.02289 AFIX 13 H112 2 0.098254 0.401756 0.765260 -21.00000 -1.20000 AFIX 0 C113 1 0.307545 0.216736 0.806511 -21.00000 0.14933 0.13777 = 0.10092 -0.04148 0.01837 -0.00157 AFIX 23 H11A 2 0.442235 0.271508 0.778927 -21.00000 -1.20000 H11B 2 0.332202 0.129696 0.780219 -21.00000 -1.20000 AFIX 0 C114 1 0.280709 0.185164 0.925794 -21.00000 0.14077 0.12765 = 0.09202 -0.04036 -0.02999 0.01668 AFIX 23 H11C 2 0.347981 0.254861 0.953481 -21.00000 -1.20000 H11D 2 0.366421 0.088809 0.958873 -21.00000 -1.20000 AFIX 0 C115 1 0.005289 0.196799 0.946739 -21.00000 0.14300 0.13196 = 0.09478 -0.04224 -0.00934 0.00928 AFIX 23 H11E 2 -0.044431 0.104117 0.950967 -21.00000 -1.20000 H11F 2 -0.036094 0.220330 1.015933 -21.00000 -1.20000 AFIX 0 C116 1 -0.092257 0.308926 0.687867 -21.00000 0.11944 0.16303 = 0.12097 0.02850 -0.04438 -0.03725 AFIX 137 H11G 2 -0.083925 0.213068 0.678393 -21.00000 -1.50000 H11H 2 -0.027642 0.368895 0.623644 -21.00000 -1.50000 H11I 2 -0.263882 0.348551 0.701091 -21.00000 -1.50000 AFIX 0 HKLF 4 REM ohd492_5_numabs_a.res in P-1 REM R1 = 0.0373 for 2470 Fo > 4sig(Fo) and 0.0413 for all 2742 data REM 241 parameters refined using 132 restraints END WGHT 0.0687 0.3722 REM Highest difference peak 0.982, deepest hole -0.696, 1-sigma level 0.112 Q1 1 -0.2214 0.5018 1.0223 11.00000 0.05 0.98 Q2 1 -0.1718 0.4202 0.9258 11.00000 0.05 0.94 Q3 1 -0.2209 0.6033 0.9629 11.00000 0.05 0.82 Q4 1 -0.1870 0.5357 0.8536 11.00000 0.05 0.82 Q5 1 0.1383 0.2195 0.7449 11.00000 0.05 0.71 Q6 1 0.0934 0.2768 0.7777 11.00000 0.05 0.64 Q7 1 0.1901 0.2364 0.7749 11.00000 0.05 0.62 Q8 1 0.0404 0.1895 0.8578 11.00000 0.05 0.59 Q9 1 -0.1940 0.1312 0.7659 11.00000 0.05 0.49 Q10 1 0.2101 0.0771 0.9682 11.00000 0.05 0.45 Q11 1 -0.2074 0.3473 0.8142 11.00000 0.05 0.43 Q12 1 -0.1948 0.1173 0.8538 11.00000 0.05 0.40 Q13 1 -0.2473 0.3948 0.7350 11.00000 0.05 0.34 Q14 1 -0.2449 0.2870 0.7531 11.00000 0.05 0.34 Q15 1 0.2087 0.3545 0.7784 11.00000 0.05 0.34 Q16 1 -0.2223 0.4183 0.7193 11.00000 0.05 0.33 Q17 1 -0.2371 0.4077 0.9919 11.00000 0.05 0.33 Q18 1 0.3683 0.5269 0.9026 11.00000 0.05 0.32 Q19 1 -0.2262 0.6414 0.8807 11.00000 0.05 0.30 Q20 1 0.0432 0.0699 0.8808 11.00000 0.05 0.28 ; _shelx_res_checksum 81970 _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 - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.747 _oxdiff_exptl_absorpt_empirical_full_min 0.637 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 -0.20288(4) 0.51237(4) 0.93359(2) 0.05543(15) Uani 1 1 d . . . . . F20 F 0.2479(7) 0.5945(5) 0.6137(2) 0.0959(12) Uani 1 1 d . . . . . F21 F 0.5355(10) 0.7124(6) 0.4534(3) 0.1207(17) Uani 1 1 d . . . . . F22 F 0.8170(7) 0.8976(5) 0.4791(3) 0.0984(11) Uani 1 1 d . . . . . F23 F 0.8110(8) 0.9651(4) 0.6685(3) 0.0982(12) Uani 1 1 d . . . . . F24 F 0.5320(6) 0.8436(3) 0.8304(2) 0.0738(8) Uani 1 1 d . . . . . O11 O 0.0140(5) 0.6457(4) 0.8107(2) 0.0616(8) Uani 1 1 d . . . . . O13 O 0.3591(5) 0.5743(3) 0.9028(2) 0.0549(7) Uani 1 1 d . . . . . O101 O -0.037(2) 0.2858(12) 0.8971(7) 0.109(3) Uani 0.640(10) 1 d D U P A 1 O111 O -0.136(4) 0.308(2) 0.8621(17) 0.121(5) Uani 0.360(10) 1 d D U P A 2 C12 C 0.2396(6) 0.6383(4) 0.8224(3) 0.0466(8) Uani 1 1 d . . . . . C14 C 0.3822(6) 0.7144(4) 0.7284(3) 0.0476(8) Uani 1 1 d . . . . . C15 C 0.3852(9) 0.6854(6) 0.6303(4) 0.0634(11) Uani 1 1 d . . . . . C16 C 0.5310(11) 0.7475(7) 0.5469(4) 0.0748(14) Uani 1 1 d . . . . . C17 C 0.6749(9) 0.8390(6) 0.5604(4) 0.0687(13) Uani 1 1 d . . . . . C18 C 0.6709(9) 0.8731(5) 0.6548(4) 0.0644(12) Uani 1 1 d . . . . . C19 C 0.5265(8) 0.8094(5) 0.7381(3) 0.0532(9) Uani 1 1 d . . . . . C102 C -0.058(3) 0.2368(16) 0.8070(10) 0.123(3) Uani 0.640(10) 1 d D . P A 1 H102 H -0.1845 0.1732 0.8264 0.147 Uiso 0.640(10) 1 calc R . P A 1 C103 C 0.173(3) 0.1452(17) 0.7906(10) 0.123(3) Uani 0.640(10) 1 d D U P A 1 H10A H 0.2859 0.1984 0.7403 0.147 Uiso 0.640(10) 1 calc R . P A 1 H10B H 0.1424 0.0644 0.7643 0.147 Uiso 0.640(10) 1 calc R . P A 1 C104 C 0.274(3) 0.0960(15) 0.9020(10) 0.121(4) Uani 0.640(10) 1 d D U P A 1 H10C H 0.2382 -0.0002 0.9360 0.145 Uiso 0.640(10) 1 calc R . P A 1 H10D H 0.4543 0.0926 0.8987 0.145 Uiso 0.640(10) 1 calc R . P A 1 C105 C 0.155(3) 0.1968(16) 0.9649(11) 0.114(4) Uani 0.640(10) 1 d D U P A 1 H10E H 0.0848 0.1463 1.0329 0.137 Uiso 0.640(10) 1 calc R . P A 1 H10F H 0.2740 0.2531 0.9796 0.137 Uiso 0.640(10) 1 calc R . P A 1 C106 C -0.169(3) 0.3620(15) 0.7188(10) 0.097(4) Uani 0.640(10) 1 d D U P A 1 H10G H -0.1427 0.4508 0.7331 0.145 Uiso 0.640(10) 1 calc GR . P A 1 H10H H -0.3465 0.3622 0.7164 0.145 Uiso 0.640(10) 1 calc GR . P A 1 H10I H -0.0904 0.3531 0.6506 0.145 Uiso 0.640(10) 1 calc GR . P A 1 C112 C 0.061(3) 0.3031(19) 0.7816(11) 0.072(3) Uani 0.360(10) 1 d D U P A 2 H112 H 0.0983 0.4018 0.7653 0.086 Uiso 0.360(10) 1 calc R . P A 2 C113 C 0.308(4) 0.217(3) 0.8065(18) 0.131(6) Uani 0.360(10) 1 d D U P A 2 H11A H 0.4422 0.2715 0.7789 0.157 Uiso 0.360(10) 1 calc R . P A 2 H11B H 0.3322 0.1297 0.7802 0.157 Uiso 0.360(10) 1 calc R . P A 2 C114 C 0.281(5) 0.185(4) 0.9258(18) 0.121(5) Uani 0.360(10) 1 d D U P A 2 H11C H 0.3480 0.2549 0.9535 0.145 Uiso 0.360(10) 1 calc R . P A 2 H11D H 0.3664 0.0888 0.9589 0.145 Uiso 0.360(10) 1 calc R . P A 2 C115 C 0.005(5) 0.197(3) 0.947(2) 0.124(6) Uani 0.360(10) 1 d D U P A 2 H11E H -0.0444 0.1041 0.9510 0.149 Uiso 0.360(10) 1 calc R . P A 2 H11F H -0.0361 0.2203 1.0159 0.149 Uiso 0.360(10) 1 calc R . P A 2 C116 C -0.092(7) 0.309(4) 0.688(2) 0.142(11) Uani 0.360(10) 1 d D U P A 2 H11G H -0.0839 0.2131 0.6784 0.213 Uiso 0.360(10) 1 calc GR . P A 2 H11H H -0.0276 0.3689 0.6236 0.213 Uiso 0.360(10) 1 calc GR . P A 2 H11I H -0.2639 0.3486 0.7011 0.213 Uiso 0.360(10) 1 calc GR . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02634(17) 0.0943(3) 0.04199(18) -0.00764(14) 0.00500(11) -0.01578(13) F20 0.097(3) 0.162(3) 0.0529(16) -0.0319(19) 0.0112(16) -0.082(3) F21 0.137(4) 0.203(5) 0.0422(16) -0.034(2) 0.027(2) -0.091(4) F22 0.087(2) 0.133(3) 0.0646(19) 0.0124(18) 0.0226(17) -0.054(2) F23 0.107(3) 0.096(2) 0.099(3) -0.0095(19) 0.011(2) -0.062(2) F24 0.082(2) 0.0825(17) 0.0637(16) -0.0247(14) 0.0066(15) -0.0263(15) O11 0.0262(13) 0.104(2) 0.0445(15) 0.0027(15) -0.0018(11) -0.0151(13) O13 0.0257(12) 0.091(2) 0.0380(13) 0.0019(13) 0.0029(10) -0.0112(12) O101 0.124(6) 0.127(6) 0.064(4) -0.040(4) -0.034(4) 0.046(5) O111 0.131(11) 0.132(9) 0.105(10) -0.056(8) 0.014(8) 0.004(9) C12 0.0255(16) 0.074(2) 0.0376(17) -0.0083(16) 0.0046(13) -0.0095(15) C14 0.0273(16) 0.071(2) 0.0389(18) -0.0023(16) 0.0020(13) -0.0099(15) C15 0.050(2) 0.099(3) 0.043(2) -0.009(2) 0.0031(18) -0.032(2) C16 0.067(3) 0.118(4) 0.039(2) -0.008(2) 0.009(2) -0.036(3) C17 0.050(2) 0.094(3) 0.051(2) 0.007(2) 0.009(2) -0.023(2) C18 0.048(2) 0.069(3) 0.069(3) 0.003(2) 0.001(2) -0.019(2) C19 0.042(2) 0.066(2) 0.048(2) -0.0061(17) 0.0004(16) -0.0087(17) C102 0.142(8) 0.133(7) 0.100(6) -0.056(5) 0.007(6) -0.007(6) C103 0.142(8) 0.133(7) 0.100(6) -0.056(5) 0.007(6) -0.007(6) C104 0.145(9) 0.112(7) 0.099(7) -0.037(6) -0.021(7) 0.021(7) C105 0.135(9) 0.114(6) 0.081(6) -0.038(5) -0.038(6) 0.048(7) C106 0.097(9) 0.122(9) 0.080(7) -0.047(6) -0.039(6) 0.004(6) C112 0.073(7) 0.097(7) 0.055(6) -0.036(6) 0.015(5) -0.023(6) C113 0.149(11) 0.138(10) 0.101(9) -0.041(9) 0.018(9) -0.002(10) C114 0.141(11) 0.128(10) 0.092(10) -0.040(9) -0.030(9) 0.017(10) C115 0.143(11) 0.132(10) 0.095(10) -0.042(8) -0.009(10) 0.009(11) C116 0.119(19) 0.16(2) 0.121(19) 0.028(17) -0.044(16) -0.037(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 0 8 0.0076 0 0 -8 0.0076 0 -6 -2 0.0093 0 6 2 0.0113 -4 -2 -1 0.0763 4 1 1 0.0829 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 Ag1 84.44(7) . 2_567 ? O11 Ag1 O13 111.93(10) . 1_455 ? O11 Ag1 O13 156.85(13) . 2_567 ? O11 Ag1 O101 98.0(3) . . ? O11 Ag1 O111 97.4(5) . . ? O13 Ag1 Ag1 149.41(7) 1_455 2_567 ? O13 Ag1 Ag1 77.49(7) 2_567 2_567 ? O13 Ag1 O13 78.96(10) 2_567 1_455 ? O13 Ag1 O101 96.6(3) 2_567 . ? O13 Ag1 O111 101.7(5) 2_567 . ? O101 Ag1 Ag1 90.6(2) . 2_567 ? O101 Ag1 O13 111.4(3) . 1_455 ? O111 Ag1 Ag1 107.3(6) . 2_567 ? O111 Ag1 O13 96.4(6) . 1_455 ? C12 O11 Ag1 119.6(3) . . ? Ag1 O13 Ag1 101.04(10) 2_567 1_655 ? C12 O13 Ag1 132.4(2) . 1_655 ? C12 O13 Ag1 126.5(2) . 2_567 ? C102 O101 Ag1 129.7(7) . . ? C102 O101 C105 111.8(9) . . ? C105 O101 Ag1 117.0(7) . . ? C112 O111 Ag1 115.9(14) . . ? C112 O111 C115 94.6(17) . . ? C115 O111 Ag1 102.8(16) . . ? O11 C12 C14 116.4(3) . . ? O13 C12 O11 126.9(4) . . ? O13 C12 C14 116.6(3) . . ? C15 C14 C12 121.8(4) . . ? C19 C14 C12 121.5(4) . . ? C19 C14 C15 116.6(4) . . ? F20 C15 C14 120.4(4) . . ? F20 C15 C16 118.2(4) . . ? C14 C15 C16 121.4(4) . . ? F21 C16 C15 119.5(5) . . ? F21 C16 C17 120.2(5) . . ? C17 C16 C15 120.2(5) . . ? F22 C17 C16 119.6(5) . . ? F22 C17 C18 120.5(5) . . ? C18 C17 C16 120.0(4) . . ? F23 C18 C17 120.3(4) . . ? F23 C18 C19 120.2(5) . . ? C17 C18 C19 119.5(4) . . ? F24 C19 C14 120.1(4) . . ? F24 C19 C18 117.5(4) . . ? C14 C19 C18 122.4(4) . . ? O101 C102 H102 105.6 . . ? O101 C102 C103 108.4(11) . . ? O101 C102 C106 108.6(10) . . ? C103 C102 H102 105.6 . . ? C103 C102 C106 121.9(13) . . ? C106 C102 H102 105.6 . . ? C102 C103 H10A 111.4 . . ? C102 C103 H10B 111.4 . . ? C102 C103 C104 101.8(10) . . ? H10A C103 H10B 109.3 . . ? C104 C103 H10A 111.4 . . ? C104 C103 H10B 111.4 . . ? C103 C104 H10C 109.9 . . ? C103 C104 H10D 109.9 . . ? H10C C104 H10D 108.3 . . ? C105 C104 C103 108.8(10) . . ? C105 C104 H10C 109.9 . . ? C105 C104 H10D 109.9 . . ? O101 C105 C104 103.4(9) . . ? O101 C105 H10E 111.1 . . ? O101 C105 H10F 111.1 . . ? C104 C105 H10E 111.1 . . ? C104 C105 H10F 111.1 . . ? H10E C105 H10F 109.1 . . ? C102 C106 H10G 109.5 . . ? C102 C106 H10H 109.5 . . ? C102 C106 H10I 109.5 . . ? H10G C106 H10H 109.5 . . ? H10G C106 H10I 109.5 . . ? H10H C106 H10I 109.5 . . ? O111 C112 H112 101.9 . . ? O111 C112 C113 122.0(17) . . ? O111 C112 C116 99(2) . . ? C113 C112 H112 101.9 . . ? C113 C112 C116 126(2) . . ? C116 C112 H112 101.9 . . ? C112 C113 H11A 112.2 . . ? C112 C113 H11B 112.2 . . ? C112 C113 C114 97.8(17) . . ? H11A C113 H11B 109.8 . . ? C114 C113 H11A 112.2 . . ? C114 C113 H11B 112.2 . . ? C113 C114 H11C 111.0 . . ? C113 C114 H11D 111.0 . . ? C113 C114 C115 104(2) . . ? H11C C114 H11D 109.0 . . ? C115 C114 H11C 111.0 . . ? C115 C114 H11D 111.0 . . ? O111 C115 C114 112(2) . . ? O111 C115 H11E 109.2 . . ? O111 C115 H11F 109.2 . . ? C114 C115 H11E 109.2 . . ? C114 C115 H11F 109.2 . . ? H11E C115 H11F 107.9 . . ? C112 C116 H11G 109.5 . . ? C112 C116 H11H 109.5 . . ? C112 C116 H11I 109.5 . . ? H11G C116 H11H 109.5 . . ? H11G C116 H11I 109.5 . . ? H11H C116 H11I 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 Ag1 2.8681(5) 2_567 ? Ag1 O11 2.225(3) . ? Ag1 O13 2.259(3) 2_567 ? Ag1 O13 2.423(3) 1_455 ? Ag1 O101 2.419(10) . ? Ag1 O111 2.40(2) . ? F20 C15 1.339(6) . ? F21 C16 1.349(7) . ? F22 C17 1.343(5) . ? F23 C18 1.345(6) . ? F24 C19 1.335(5) . ? O11 C12 1.252(5) . ? O13 Ag1 2.259(3) 2_567 ? O13 Ag1 2.423(3) 1_655 ? O13 C12 1.246(5) . ? O101 C102 1.399(13) . ? O101 C105 1.444(12) . ? O111 C112 1.458(16) . ? O111 C115 1.495(19) . ? C12 C14 1.513(5) . ? C14 C15 1.380(6) . ? C14 C19 1.368(6) . ? C15 C16 1.384(6) . ? C16 C17 1.355(8) . ? C17 C18 1.354(8) . ? C18 C19 1.385(6) . ? C102 H102 1.0000 . ? C102 C103 1.461(9) . ? C102 C106 1.532(15) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C103 C104 1.523(14) . ? C104 H10C 0.9900 . ? C104 H10D 0.9900 . ? C104 C105 1.484(9) . ? C105 H10E 0.9900 . ? C105 H10F 0.9900 . ? C106 H10G 0.9800 . ? C106 H10H 0.9800 . ? C106 H10I 0.9800 . ? C112 H112 1.0000 . ? C112 C113 1.485(10) . ? C112 C116 1.519(18) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C113 C114 1.509(18) . ? C114 H11C 0.9900 . ? C114 H11D 0.9900 . ? C114 C115 1.514(19) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C116 H11G 0.9800 . ? C116 H11H 0.9800 . ? C116 H11I 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 0.0585 0.2877 8.2786 0.0251 0.9996 -0.0091 -0.0585 -0.2877 -8.2786 -0.0251 -0.9996 0.0091 -0.0647 -6.3384 -1.8329 0.2157 -0.0083 0.9764 0.0647 6.3384 1.8329 -0.2157 0.0083 -0.9764 -3.5516 -1.9361 -0.7286 -0.9338 0.0224 0.3570 3.5781 1.4106 0.5782 0.9607 -0.0233 -0.2766