#------------------------------------------------------------------------------ #$Date: 2024-07-05 18:35:15 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292979 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248659.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_7248659 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 'C17 H16 Ag F5 O3' _chemical_formula_sum 'C17 H16 Ag F5 O3' _chemical_formula_weight 471.17 _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 2024-04-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-04-29 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.6040(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.9355(2) _cell_length_b 5.51250(10) _cell_length_c 22.5133(2) _cell_measurement_reflns_used 12522 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 76.4500 _cell_measurement_theta_min 3.6280 _cell_volume 1726.04(4) _computing_cell_refinement 'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.100a 64-bit (release 06-12-2023))' _computing_data_reduction 'CrysAlisPro 1.171.43.100a (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 120.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 32.00 98.00 0.50 0.10 -- 102.08-125.00-180.00 132 2 \w 77.00 106.00 0.50 0.10 -- 102.08-125.00 -90.00 58 3 \w 32.00 96.00 0.50 0.10 -- 102.08-125.00 150.00 128 4 \w 36.00 134.00 0.50 0.10 -- 102.08-158.00 165.00 196 5 \w 36.00 134.00 0.50 0.10 -- 102.08-158.00 165.00 196 6 \w 37.00 63.00 0.50 0.10 -- 102.08 -99.00 30.00 52 7 \w 77.00 104.00 0.50 0.10 -- 102.08 -99.00 0.00 54 8 \w 73.00 105.00 0.50 0.10 -- 102.08 -99.00 30.00 64 9 \w 15.00 100.00 0.50 0.05 -- 52.06-119.00 -40.00 170 10 \w 33.00 109.00 0.50 0.10 -- 102.08-119.00 -40.00 152 11 \w 74.00 104.00 0.50 0.10 -- 102.08 -99.00 -60.00 60 12 \w 32.00 78.00 0.50 0.10 -- 102.08 -57.00 -30.00 92 13 \w 25.00 50.00 0.50 0.10 -- 102.08 -38.00 -90.00 50 14 \w 30.00 78.00 0.50 0.10 -- 102.08 -57.00-150.00 96 15 \w 25.00 51.00 0.50 0.10 -- 102.08 -38.00 0.00 52 16 \w 25.00 50.00 0.50 0.10 -- 102.08 -38.00 90.00 50 17 \w 25.00 50.00 0.50 0.10 -- 102.08 -38.00 150.00 50 18 \w 25.00 50.00 0.50 0.10 -- 102.08 -38.00 120.00 50 19 \w 110.00 169.00 0.50 0.10 -- 102.08 19.00 -30.00 118 20 \w 58.00 160.00 0.50 0.10 -- 102.08 158.00-160.00 204 21 \w 58.00 119.00 0.50 0.05 -- 52.06 158.00-160.00 122 22 \w -11.00 22.00 0.50 0.05 -- 26.00 99.00-109.47 66 23 \w -4.00 25.00 0.50 0.05 -- -51.81 19.00 60.00 58 24 \w -4.00 25.00 0.50 0.05 -- -51.81 19.00 150.00 58 25 \w -48.00 -14.00 0.50 0.10 -- -87.66 57.00 60.00 68 26 \w -54.00 -29.00 0.50 0.10 -- -87.66 57.00 30.00 50 27 \w -43.00 -17.00 0.50 0.10 -- -87.66 57.00-180.00 52 28 \w -152.00 -62.00 0.50 0.10 -- -82.00 -69.00 -12.79 180 29 \w -157.00 -78.00 0.50 0.10 -- -87.66-119.00 -40.00 158 30 \w -118.00 -51.00 0.50 0.05 -- -51.81-158.00 165.00 134 31 \w -154.00 -51.00 0.50 0.10 -- -87.66-158.00 165.00 206 32 \w -100.00 -9.00 0.50 0.05 -- -51.81 119.00 44.00 182 33 \w -109.00 -38.00 0.50 0.10 -- -87.66 119.00 44.00 142 ; _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 -0.0034282000 _diffrn_orient_matrix_UB_12 0.2768976000 _diffrn_orient_matrix_UB_13 -0.0091372000 _diffrn_orient_matrix_UB_21 0.1104187000 _diffrn_orient_matrix_UB_22 0.0110667000 _diffrn_orient_matrix_UB_23 0.0090966000 _diffrn_orient_matrix_UB_31 0.0083701000 _diffrn_orient_matrix_UB_32 -0.0361042000 _diffrn_orient_matrix_UB_33 -0.0673275000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0340 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 22007 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.463 _diffrn_reflns_theta_min 3.631 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.998 _exptl_absorpt_correction_T_max 0.67245 _exptl_absorpt_correction_T_min 0.64974 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.100a (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 1.813 _exptl_crystal_description plate _exptl_crystal_F_000 936 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Dihydrocarvone:acetone (1:1)/pentane' _exptl_crystal_size_max 0.222 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.014 _exptl_crystal_size_rad 0.029 _refine_diff_density_max 0.547 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 3513 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0266 _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^)+(0.0206P)^2^+1.5439P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0602 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3104 _reflns_number_total 3513 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_Dihydrocarvone _cod_depositor_comments 'Adding full bibliography for 7248652--7248666.cif.' _cod_database_code 7248659 _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 0.907 _shelx_estimated_absorpt_t_min 0.217 _diffrn_oxdiff_digest_frames ; 014694088ba3316017572da3339c84a14303500dd92 ; _diffrn_oxdiff_digest_hkl ; 01ba60fd63fb9433e70ec09a34f94711e6b2d2 ; _reflns_odcompleteness_completeness 99.80 _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.a Ternary CH refined with riding coordinates: C103(H103), C106(H106) 2.b Secondary CH2 refined with riding coordinates: C104(H10A,H10B), C105(H10C,H10D), C107(H10E,H10F) 2.c X=CH2 refined with riding coordinates: C110(H11A,H11B) 2.d Idealised Me refined as rotating group: C108(H10G,H10H,H10I), C111(H11C,H11D,H11E) ; _shelx_res_file ; TITL ohd494_9_scale2_a.res in P2(1)/n REM Old TITL OHD494_9_scale2 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.111, Rweak 0.099, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C16 O4 F5 Ag CELL 1.54184 13.9355 5.5125 22.5133 90 93.604 90 ZERR 4 0.0002 0.0001 0.0002 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ag F O UNIT 68 64 4 20 12 L.S. 4 0 0 PLAN 20 SIZE 0.01 0.04 0.22 TEMP -153.15 BOND $H list 4 fmap 2 53 ACTA SHEL 50 0.8 REM REM REM WGHT 0.020600 1.543900 FVAR 0.40960 AG1 3 0.490343 0.293723 0.537118 11.00000 0.03747 0.01761 = 0.02116 -0.00065 -0.00011 -0.00229 F20 4 0.443225 0.746983 0.702628 11.00000 0.04312 0.05771 = 0.03462 -0.00551 0.01019 -0.01377 F21 4 0.471647 1.045745 0.795963 11.00000 0.06231 0.09958 = 0.03182 -0.02090 0.01133 0.00549 F22 4 0.615281 1.381209 0.797835 11.00000 0.08394 0.06325 = 0.04582 -0.03530 -0.02053 0.00864 F23 4 0.731962 1.405028 0.706091 11.00000 0.07812 0.04590 = 0.05710 -0.00965 -0.01940 -0.02925 F24 4 0.706749 1.101409 0.613470 11.00000 0.04743 0.04621 = 0.03506 0.00144 0.00195 -0.02132 O11 5 0.541492 0.538803 0.608810 11.00000 0.04543 0.01651 = 0.02433 0.00009 -0.00295 -0.00386 O13 5 0.549205 0.868699 0.551170 11.00000 0.03945 0.01977 = 0.01878 -0.00044 -0.00299 -0.00009 O101 5 0.361472 0.168349 0.602472 11.00000 0.03788 0.04566 = 0.03356 -0.00054 0.00283 -0.01131 C12 1 0.553543 0.758342 0.600344 11.00000 0.02574 0.01927 = 0.02132 -0.00188 -0.00201 -0.00067 C14 1 0.574230 0.915400 0.654723 11.00000 0.03107 0.01979 = 0.02251 -0.00015 -0.00414 0.00135 C15 1 0.516506 0.905211 0.702549 11.00000 0.03396 0.03461 = 0.02401 -0.00322 -0.00198 -0.00079 C16 1 0.529626 1.060317 0.750697 11.00000 0.04282 0.05456 = 0.02326 -0.00939 -0.00090 0.00931 C17 1 0.601548 1.228193 0.751468 11.00000 0.05284 0.03848 = 0.03067 -0.01572 -0.01458 0.01116 C18 1 0.661148 1.242565 0.705197 11.00000 0.04856 0.02209 = 0.03906 -0.00138 -0.01754 -0.00415 C19 1 0.646577 1.085050 0.657670 11.00000 0.03740 0.02528 = 0.02715 0.00322 -0.00635 -0.00078 C102 1 0.301414 0.006955 0.602536 11.00000 0.03063 0.03911 = 0.03079 0.00120 0.00159 0.00059 C103 1 0.230594 -0.007441 0.650572 11.00000 0.04056 0.03828 = 0.03263 0.00224 0.00794 -0.00017 AFIX 13 H103 2 0.241177 -0.165391 0.671828 11.00000 -1.20000 AFIX 0 C104 1 0.129437 -0.010622 0.620880 11.00000 0.03641 0.04045 = 0.05158 -0.00251 0.01150 -0.00155 AFIX 23 H10A 2 0.082559 -0.033283 0.651679 11.00000 -1.20000 H10B 2 0.116047 0.147950 0.601445 11.00000 -1.20000 AFIX 0 C105 1 0.115826 -0.211206 0.574686 11.00000 0.03096 0.03576 = 0.04864 0.00057 0.00626 -0.00579 AFIX 23 H10C 2 0.049677 -0.203531 0.555980 11.00000 -1.20000 H10D 2 0.124178 -0.370867 0.594473 11.00000 -1.20000 AFIX 0 C106 1 0.188573 -0.186631 0.526332 11.00000 0.03306 0.03361 = 0.04056 0.00215 0.00159 -0.00358 AFIX 13 H106 2 0.177689 -0.023574 0.507640 11.00000 -1.20000 AFIX 0 C107 1 0.290958 -0.185587 0.555068 11.00000 0.03172 0.04303 = 0.03840 -0.00405 0.00458 -0.00313 AFIX 23 H10E 2 0.305896 -0.346441 0.572891 11.00000 -1.20000 H10F 2 0.337141 -0.154178 0.524298 11.00000 -1.20000 AFIX 0 C108 1 0.245373 0.195228 0.696350 11.00000 0.04977 0.04151 = 0.03527 -0.00411 0.00807 0.00179 AFIX 137 H10G 2 0.310568 0.185118 0.715216 11.00000 -1.50000 H10H 2 0.198439 0.178129 0.726722 11.00000 -1.50000 H10I 2 0.236607 0.352665 0.676529 11.00000 -1.50000 AFIX 0 C109 1 0.172370 -0.372298 0.477078 11.00000 0.03597 0.03506 = 0.03353 0.00467 -0.00081 -0.00817 C110 1 0.228854 -0.559947 0.468893 11.00000 0.05011 0.03798 = 0.03670 -0.00108 -0.00100 -0.00346 AFIX 93 H11A 2 0.215742 -0.665070 0.435942 11.00000 -1.20000 H11B 2 0.282626 -0.589898 0.495953 11.00000 -1.20000 AFIX 0 C111 1 0.086570 -0.318563 0.435293 11.00000 0.04797 0.05130 = 0.05461 0.00695 -0.01094 -0.00547 AFIX 137 H11C 2 0.028119 -0.321872 0.457316 11.00000 -1.50000 H11D 2 0.081778 -0.441116 0.403712 11.00000 -1.50000 H11E 2 0.093891 -0.157681 0.417617 11.00000 -1.50000 AFIX 0 HKLF 4 REM ohd494_9_scale2_a.res in P2(1)/n REM R1 = 0.0266 for 3104 Fo > 4sig(Fo) and 0.0317 for all 3513 data REM 237 parameters refined using 0 restraints END WGHT 0.0206 1.5307 REM Highest difference peak 0.547, deepest hole -0.533, 1-sigma level 0.076 Q1 1 0.4984 0.5460 0.5251 11.00000 0.05 0.55 Q2 1 0.2006 0.1130 0.6264 11.00000 0.05 0.43 Q3 1 0.4902 1.0199 0.5344 11.00000 0.05 0.42 Q4 1 0.2535 -0.0419 0.5320 11.00000 0.05 0.40 Q5 1 0.4328 0.2854 0.5692 11.00000 0.05 0.39 Q6 1 0.1680 -0.1360 0.6405 11.00000 0.05 0.37 Q7 1 0.4775 0.4683 0.5817 11.00000 0.05 0.35 Q8 1 0.2223 -0.2954 0.5479 11.00000 0.05 0.34 Q9 1 0.2879 0.1191 0.5815 11.00000 0.05 0.33 Q10 1 0.2144 0.1772 0.6394 11.00000 0.05 0.32 Q11 1 0.5436 0.9219 0.6786 11.00000 0.05 0.29 Q12 1 0.5408 0.2989 0.5003 11.00000 0.05 0.28 Q13 1 0.6157 0.9862 0.6596 11.00000 0.05 0.27 Q14 1 0.6390 1.2125 0.7397 11.00000 0.05 0.26 Q15 1 0.6753 1.0730 0.6421 11.00000 0.05 0.26 Q16 1 0.3997 0.2921 0.5225 11.00000 0.05 0.26 Q17 1 0.4160 0.1027 0.5342 11.00000 0.05 0.25 Q18 1 0.2170 -0.4126 0.4596 11.00000 0.05 0.24 Q19 1 0.5905 0.3000 0.5360 11.00000 0.05 0.24 Q20 1 0.0380 -0.5048 0.4996 11.00000 0.05 0.23 ; _shelx_res_checksum 87171 _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 2.066 _oxdiff_exptl_absorpt_empirical_full_min 0.547 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 0.49034(2) 0.29372(3) 0.53712(2) 0.02550(7) Uani 1 1 d . . . . . F20 F 0.44322(13) 0.7470(4) 0.70263(7) 0.0448(5) Uani 1 1 d . . . . . F21 F 0.47165(15) 1.0457(5) 0.79596(8) 0.0642(6) Uani 1 1 d . . . . . F22 F 0.61528(17) 1.3812(4) 0.79783(8) 0.0654(6) Uani 1 1 d . . . . . F23 F 0.73196(17) 1.4050(4) 0.70609(9) 0.0614(6) Uani 1 1 d . . . . . F24 F 0.70675(13) 1.1014(4) 0.61347(7) 0.0429(4) Uani 1 1 d . . . . . O11 O 0.54149(14) 0.5388(3) 0.60881(7) 0.0290(4) Uani 1 1 d . . . . . O13 O 0.54921(13) 0.8687(3) 0.55117(7) 0.0262(4) Uani 1 1 d . . . . . O101 O 0.36147(15) 0.1683(4) 0.60247(8) 0.0390(5) Uani 1 1 d . . . . . C12 C 0.55354(18) 0.7583(5) 0.60034(10) 0.0223(5) Uani 1 1 d . . . . . C14 C 0.57423(18) 0.9154(5) 0.65472(10) 0.0247(5) Uani 1 1 d . . . . . C15 C 0.5165(2) 0.9052(6) 0.70255(11) 0.0310(6) Uani 1 1 d . . . . . C16 C 0.5296(2) 1.0603(7) 0.75070(12) 0.0403(8) Uani 1 1 d . . . . . C17 C 0.6015(2) 1.2282(6) 0.75147(13) 0.0414(8) Uani 1 1 d . . . . . C18 C 0.6611(2) 1.2426(5) 0.70520(13) 0.0374(7) Uani 1 1 d . . . . . C19 C 0.6466(2) 1.0850(5) 0.65767(11) 0.0303(6) Uani 1 1 d . . . . . C102 C 0.3014(2) 0.0070(6) 0.60254(12) 0.0335(6) Uani 1 1 d . . . . . C103 C 0.2306(2) -0.0074(6) 0.65057(12) 0.0369(7) Uani 1 1 d . . . . . H103 H 0.2412 -0.1654 0.6718 0.044 Uiso 1 1 calc R . . . . C104 C 0.1294(2) -0.0106(7) 0.62088(14) 0.0424(7) Uani 1 1 d . . . . . H10A H 0.0826 -0.0333 0.6517 0.051 Uiso 1 1 calc R . . . . H10B H 0.1160 0.1479 0.6014 0.051 Uiso 1 1 calc R . . . . C105 C 0.1158(2) -0.2112(6) 0.57469(14) 0.0383(7) Uani 1 1 d . . . . . H10C H 0.0497 -0.2035 0.5560 0.046 Uiso 1 1 calc R . . . . H10D H 0.1242 -0.3709 0.5945 0.046 Uiso 1 1 calc R . . . . C106 C 0.1886(2) -0.1866(6) 0.52633(13) 0.0358(6) Uani 1 1 d . . . . . H106 H 0.1777 -0.0236 0.5076 0.043 Uiso 1 1 calc R . . . . C107 C 0.2910(2) -0.1856(6) 0.55507(13) 0.0376(7) Uani 1 1 d . . . . . H10E H 0.3059 -0.3464 0.5729 0.045 Uiso 1 1 calc R . . . . H10F H 0.3371 -0.1542 0.5243 0.045 Uiso 1 1 calc R . . . . C108 C 0.2454(2) 0.1952(6) 0.69635(13) 0.0420(7) Uani 1 1 d . . . . . H10G H 0.3106 0.1851 0.7152 0.063 Uiso 1 1 calc GR . . . . H10H H 0.1984 0.1781 0.7267 0.063 Uiso 1 1 calc GR . . . . H10I H 0.2366 0.3527 0.6765 0.063 Uiso 1 1 calc GR . . . . C109 C 0.1724(2) -0.3723(6) 0.47708(12) 0.0350(6) Uani 1 1 d . . . . . C110 C 0.2289(2) -0.5599(6) 0.46889(13) 0.0418(7) Uani 1 1 d . . . . . H11A H 0.2157 -0.6651 0.4359 0.050 Uiso 1 1 calc R . . . . H11B H 0.2826 -0.5899 0.4960 0.050 Uiso 1 1 calc R . . . . C111 C 0.0866(3) -0.3186(7) 0.43529(16) 0.0519(9) Uani 1 1 d . . . . . H11C H 0.0281 -0.3219 0.4573 0.078 Uiso 1 1 calc GR . . . . H11D H 0.0818 -0.4411 0.4037 0.078 Uiso 1 1 calc GR . . . . H11E H 0.0939 -0.1577 0.4176 0.078 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 0.03747(11) 0.01761(11) 0.02116(10) -0.00065(7) -0.00011(7) -0.00229(8) F20 0.0431(9) 0.0577(13) 0.0346(8) -0.0055(8) 0.0102(7) -0.0138(9) F21 0.0623(13) 0.0996(19) 0.0318(9) -0.0209(11) 0.0113(8) 0.0055(13) F22 0.0839(16) 0.0633(15) 0.0458(10) -0.0353(11) -0.0205(10) 0.0086(13) F23 0.0781(15) 0.0459(13) 0.0571(11) -0.0096(10) -0.0194(10) -0.0292(12) F24 0.0474(10) 0.0462(11) 0.0351(8) 0.0014(8) 0.0019(7) -0.0213(9) O11 0.0454(11) 0.0165(10) 0.0243(8) 0.0001(7) -0.0030(7) -0.0039(8) O13 0.0394(10) 0.0198(9) 0.0188(8) -0.0004(7) -0.0030(7) -0.0001(8) O101 0.0379(11) 0.0457(14) 0.0336(10) -0.0005(9) 0.0028(8) -0.0113(10) C12 0.0257(11) 0.0193(14) 0.0213(11) -0.0019(10) -0.0020(9) -0.0007(10) C14 0.0311(13) 0.0198(14) 0.0225(11) -0.0001(10) -0.0041(9) 0.0014(11) C15 0.0340(14) 0.0346(17) 0.0240(12) -0.0032(12) -0.0020(10) -0.0008(13) C16 0.0428(16) 0.055(2) 0.0233(13) -0.0094(14) -0.0009(11) 0.0093(15) C17 0.0528(18) 0.0385(19) 0.0307(14) -0.0157(13) -0.0146(13) 0.0112(15) C18 0.0486(17) 0.0221(16) 0.0391(15) -0.0014(12) -0.0175(13) -0.0041(13) C19 0.0374(14) 0.0253(16) 0.0272(12) 0.0032(11) -0.0063(11) -0.0008(12) C102 0.0306(13) 0.0391(18) 0.0308(13) 0.0012(12) 0.0016(11) 0.0006(13) C103 0.0406(15) 0.0383(18) 0.0326(14) 0.0022(13) 0.0079(12) -0.0002(14) C104 0.0364(15) 0.0404(19) 0.0516(18) -0.0025(15) 0.0115(13) -0.0016(14) C105 0.0310(13) 0.0358(17) 0.0486(17) 0.0006(14) 0.0063(12) -0.0058(13) C106 0.0331(14) 0.0336(17) 0.0406(15) 0.0022(13) 0.0016(12) -0.0036(13) C107 0.0317(14) 0.0430(19) 0.0384(15) -0.0040(14) 0.0046(12) -0.0031(13) C108 0.0498(18) 0.0415(19) 0.0353(14) -0.0041(14) 0.0081(13) 0.0018(16) C109 0.0360(14) 0.0351(17) 0.0335(14) 0.0047(13) -0.0008(11) -0.0082(13) C110 0.0501(18) 0.038(2) 0.0367(15) -0.0011(14) -0.0010(13) -0.0035(15) C111 0.0480(19) 0.051(2) 0.0546(19) 0.0069(17) -0.0109(15) -0.0055(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 8 0 4 0.0038 -8 0 -4 0.0098 0 4 -1 0.1102 0 -4 1 0.1102 1 0 -15 0.0234 -1 0 15 0.0144 0 -3 -4 0.1083 -1 -2 11 0.0741 0 3 9 0.0897 9 -1 -3 0.0350 9 0 -4 0.0089 1 3 -10 0.0947 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 84.34(5) . 3_666 ? O11 Ag1 O13 163.92(7) . 3_666 ? O11 Ag1 O13 113.37(6) . 1_545 ? O11 Ag1 O101 87.08(7) . . ? O13 Ag1 Ag1 141.48(4) 1_545 3_666 ? O13 Ag1 Ag1 79.84(5) 3_666 3_666 ? O13 Ag1 O13 78.22(7) 3_666 1_545 ? O13 Ag1 O101 105.65(7) 3_666 . ? O101 Ag1 Ag1 131.86(6) . 3_666 ? O101 Ag1 O13 84.72(7) . 1_545 ? C12 O11 Ag1 122.05(16) . . ? Ag1 O13 Ag1 101.78(7) 3_666 1_565 ? C12 O13 Ag1 125.97(16) . 3_666 ? C12 O13 Ag1 124.14(15) . 1_565 ? C102 O101 Ag1 136.26(18) . . ? O11 C12 O13 127.4(2) . . ? O11 C12 C14 117.1(2) . . ? O13 C12 C14 115.5(2) . . ? C15 C14 C12 121.0(2) . . ? C19 C14 C12 122.1(2) . . ? C19 C14 C15 116.8(2) . . ? F20 C15 C14 120.4(2) . . ? F20 C15 C16 117.6(2) . . ? C16 C15 C14 122.0(3) . . ? F21 C16 C15 120.1(3) . . ? F21 C16 C17 120.5(3) . . ? C17 C16 C15 119.4(3) . . ? F22 C17 C16 120.2(3) . . ? F22 C17 C18 119.2(3) . . ? C16 C17 C18 120.5(3) . . ? F23 C18 C17 120.6(3) . . ? F23 C18 C19 120.4(3) . . ? C17 C18 C19 118.9(3) . . ? F24 C19 C14 120.0(2) . . ? F24 C19 C18 117.6(3) . . ? C14 C19 C18 122.4(3) . . ? O101 C102 C103 121.2(3) . . ? O101 C102 C107 123.2(2) . . ? C107 C102 C103 115.6(3) . . ? C102 C103 H103 107.7 . . ? C102 C103 C104 108.4(2) . . ? C102 C103 C108 112.2(3) . . ? C104 C103 H103 107.7 . . ? C104 C103 C108 112.8(3) . . ? C108 C103 H103 107.7 . . ? C103 C104 H10A 109.1 . . ? C103 C104 H10B 109.1 . . ? H10A C104 H10B 107.9 . . ? C105 C104 C103 112.4(3) . . ? C105 C104 H10A 109.1 . . ? C105 C104 H10B 109.1 . . ? C104 C105 H10C 109.4 . . ? C104 C105 H10D 109.4 . . ? C104 C105 C106 111.1(3) . . ? H10C C105 H10D 108.0 . . ? C106 C105 H10C 109.4 . . ? C106 C105 H10D 109.4 . . ? C105 C106 H106 106.7 . . ? C107 C106 C105 109.9(2) . . ? C107 C106 H106 106.7 . . ? C109 C106 C105 112.6(3) . . ? C109 C106 H106 106.7 . . ? C109 C106 C107 113.8(3) . . ? C102 C107 C106 110.4(2) . . ? C102 C107 H10E 109.6 . . ? C102 C107 H10F 109.6 . . ? C106 C107 H10E 109.6 . . ? C106 C107 H10F 109.6 . . ? H10E C107 H10F 108.1 . . ? C103 C108 H10G 109.5 . . ? C103 C108 H10H 109.5 . . ? C103 C108 H10I 109.5 . . ? H10G C108 H10H 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C110 C109 C106 124.7(3) . . ? C110 C109 C111 121.7(3) . . ? C111 C109 C106 113.6(3) . . ? C109 C110 H11A 120.0 . . ? C109 C110 H11B 120.0 . . ? H11A C110 H11B 120.0 . . ? C109 C111 H11C 109.5 . . ? C109 C111 H11D 109.5 . . ? C109 C111 H11E 109.5 . . ? H11C C111 H11D 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 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 2.8450(4) 3_666 ? Ag1 O11 2.1895(18) . ? Ag1 O13 2.2178(16) 3_666 ? Ag1 O13 2.4959(19) 1_545 ? Ag1 O101 2.4900(19) . ? F20 C15 1.343(3) . ? F21 C16 1.342(3) . ? F22 C17 1.346(3) . ? F23 C18 1.332(4) . ? F24 C19 1.344(3) . ? O11 C12 1.238(3) . ? O13 Ag1 2.4959(19) 1_565 ? O13 Ag1 2.2177(16) 3_666 ? O13 C12 1.261(3) . ? O101 C102 1.222(4) . ? C12 C14 1.512(3) . ? C14 C15 1.385(4) . ? C14 C19 1.374(4) . ? C15 C16 1.384(4) . ? C16 C17 1.363(5) . ? C17 C18 1.375(5) . ? C18 C19 1.383(4) . ? C102 C103 1.511(4) . ? C102 C107 1.507(4) . ? C103 H103 1.0000 . ? C103 C104 1.522(4) . ? C103 C108 1.525(4) . ? C104 H10A 0.9900 . ? C104 H10B 0.9900 . ? C104 C105 1.522(5) . ? C105 H10C 0.9900 . ? C105 H10D 0.9900 . ? C105 C106 1.539(4) . ? C106 H106 1.0000 . ? C106 C107 1.529(4) . ? C106 C109 1.515(4) . ? C107 H10E 0.9900 . ? C107 H10F 0.9900 . ? C108 H10G 0.9800 . ? C108 H10H 0.9800 . ? C108 H10I 0.9800 . ? C109 C110 1.320(5) . ? C109 C111 1.504(4) . ? C110 H11A 0.9500 . ? C110 H11B 0.9500 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 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 8.4339 -0.0275 4.4171 -0.0769 0.9711 -0.2258 -8.4339 0.0275 -4.4171 0.0769 -0.9711 0.2258 0.4347 3.5688 -0.8565 0.9945 0.0797 -0.0675 -0.4347 -3.5688 0.8565 -0.9945 -0.0797 0.0675 1.2598 -0.0506 -14.5706 0.1148 0.0060 0.9934 -1.2598 0.0506 14.5706 -0.1148 -0.0060 -0.9934 0.0002 -2.9977 -3.9807 -0.7937 -0.0694 0.3762 -1.0145 -1.9975 11.0036 -0.6502 -0.0340 -0.6772 -0.0068 2.9978 8.9776 0.7481 0.1141 -0.7127 8.9713 -1.0038 -2.9856 -0.2814 0.9523 0.3123 8.9743 -0.0046 -3.9905 0.0044 0.9546 0.3440 1.0149 2.9967 -10.0099 0.9178 0.0542 0.5742