#------------------------------------------------------------------------------ #$Date: 2024-05-21 01:38:30 +0300 (Tue, 21 May 2024) $ #$Revision: 291962 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/86/7248660.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_7248660 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 'C32 H20 Ag2 F10 O6, 2(C9 H10 O)' _chemical_formula_sum 'C50 H40 Ag2 F10 O8' _chemical_formula_weight 1174.56 _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 2024-02-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-02-23 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _cell_angle_alpha 85.841(4) _cell_angle_beta 85.713(3) _cell_angle_gamma 84.263(3) _cell_formula_units_Z 1 _cell_length_a 7.2534(3) _cell_length_b 11.0121(5) _cell_length_c 13.8225(6) _cell_measurement_reflns_used 12381 _cell_measurement_temperature 120.00(11) _cell_measurement_theta_max 76.2500 _cell_measurement_theta_min 3.1970 _cell_volume 1093.11(8) _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(11) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -54.00 -13.00 0.50 0.10 -- -87.66 57.00 60.00 82 2 \w -112.00 -36.00 0.50 0.10 -- -87.66 77.00-150.00 152 3 \w -112.00 -36.00 0.50 0.10 -- -87.66 77.00-150.00 152 4 \w -58.00 -14.00 0.50 0.10 -- -87.66 59.00-166.00 88 5 \w -58.00 22.00 0.50 0.05 -- -51.43 59.00-166.00 160 6 \w -4.00 25.00 0.50 0.05 -- -51.43 19.00 -90.00 58 7 \w -54.00 -13.00 0.50 0.10 -- -87.66 57.00 120.00 82 8 \w -4.00 25.00 0.50 0.05 -- -51.43 19.00 120.00 58 9 \w 63.00 106.00 0.50 0.10 -- 102.08 19.00-180.00 86 10 \w 85.00 176.00 0.50 0.10 -- 102.08 59.00-166.00 182 11 \w 83.00 161.00 0.50 0.10 -- 102.08 77.00-150.00 156 12 \w 34.00 126.00 0.50 0.05 -- 51.81 59.00-166.00 184 13 \w 34.00 126.00 0.50 0.05 -- 51.81 59.00-166.00 184 14 \w 129.00 165.00 0.50 0.10 -- 102.08 19.00-180.00 72 15 \w 85.00 176.00 0.50 0.10 -- 102.08 59.00-166.00 182 16 \w 126.00 152.00 0.50 0.10 -- 102.08 57.00 -60.00 52 17 \w 122.00 168.00 0.50 0.10 -- 102.08 77.00 120.00 92 18 \w 78.00 113.00 0.50 0.10 -- 102.08 77.00 120.00 70 19 \w 119.00 168.00 0.50 0.10 -- 102.08 125.00 120.00 98 20 \w 81.00 149.00 0.50 0.10 -- 102.08 125.00 60.00 136 21 \w 81.00 152.00 0.50 0.10 -- 102.08 125.00 30.00 142 22 \w -54.00 -28.00 0.50 0.05 -- 18.00 154.00-129.49 52 23 \w 26.00 52.00 0.50 0.10 -- 102.08 -38.00 0.00 52 24 \w 29.00 73.00 0.50 0.10 -- 102.08 -57.00 0.00 88 25 \w 101.00 127.00 0.50 0.10 -- 102.08 -77.00 60.00 52 26 \w 47.00 73.00 0.50 0.10 -- 102.08 -57.00 -60.00 52 27 \w -22.00 70.00 0.50 0.05 -- 51.81 -59.00 53.00 184 28 \w 29.00 83.00 0.50 0.10 -- 102.08 -59.00 53.00 108 29 \w 35.00 70.00 0.50 0.10 -- 102.08 -77.00 60.00 70 30 \w 68.00 110.00 0.50 0.10 -- 102.08-125.00 60.00 84 31 \w 65.00 98.00 0.50 0.10 -- 102.08 -99.00 60.00 66 32 \w 34.00 59.00 0.50 0.10 -- 102.08-125.00 60.00 50 33 \w 35.00 102.00 0.50 0.10 -- 102.08 -99.00 -30.00 134 34 \w 34.00 90.00 0.50 0.10 -- 102.08-125.00 -30.00 112 35 \w 38.00 67.00 0.50 0.10 -- 102.08 -99.00 -90.00 58 36 \w 71.00 106.00 0.50 0.10 -- 102.08 -99.00 -90.00 70 37 \w 74.00 106.00 0.50 0.10 -- 102.08 -99.00-150.00 64 38 \w 68.00 94.00 0.50 0.10 -- 102.08 -99.00-120.00 52 39 \w 44.00 69.00 0.50 0.10 -- 102.08 -99.00-150.00 50 40 \w 36.00 66.00 0.50 0.10 -- 102.08 -99.00-120.00 60 41 \w 35.00 96.00 0.50 0.10 -- 102.08 -99.00-180.00 122 42 \w 75.00 106.00 0.50 0.10 -- 102.08 -99.00 90.00 62 43 \w 44.00 70.00 0.50 0.10 -- 102.08 -99.00 120.00 52 44 \w 80.00 106.00 0.50 0.10 -- 102.08 -99.00 120.00 52 45 \w -112.00 -17.00 0.50 0.10 -- -87.66 125.00-150.00 190 46 \w -112.00 -17.00 0.50 0.10 -- -87.66 125.00 -60.00 190 47 \w -112.00 -17.00 0.50 0.10 -- -87.66 125.00 -60.00 190 48 \w -155.00 -86.00 0.50 0.10 -- -87.66 -99.00-180.00 138 49 \w -122.00 -74.00 0.50 0.05 -- -51.43-125.00-150.00 96 50 \w -161.00 -70.00 0.50 0.10 -- -87.66 -59.00 53.00 182 51 \w -125.00 -34.00 0.50 0.05 -- -51.43 -59.00 53.00 182 ; _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 -0.1867775000 _diffrn_orient_matrix_UB_12 -0.0427697000 _diffrn_orient_matrix_UB_13 0.0427042000 _diffrn_orient_matrix_UB_21 0.0262880000 _diffrn_orient_matrix_UB_22 -0.1083619000 _diffrn_orient_matrix_UB_23 -0.0657921000 _diffrn_orient_matrix_UB_31 0.1009997000 _diffrn_orient_matrix_UB_32 -0.0792632000 _diffrn_orient_matrix_UB_33 0.0799585000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_unetI/netI 0.0407 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 22573 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.497 _diffrn_reflns_theta_min 3.213 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.081 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.100a (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 1.784 _exptl_crystal_description plate _exptl_crystal_F_000 588 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: isochroman/pentane' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.032 _exptl_crystal_size_min 0.028 _refine_diff_density_max 1.533 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 4439 _refine_ls_number_restraints 38 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0355 _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^)+(0.0223P)^2^+1.8871P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.0793 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3829 _reflns_number_total 4439 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00441h2.cif _cod_data_source_block 1_Isochroman _cod_database_code 7248660 _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 0.805 _shelx_estimated_absorpt_t_min 0.470 _diffrn_oxdiff_digest_frames ; 0156087976f892603c4c41124f633d95ce05382900b ; _diffrn_oxdiff_digest_hkl ; 01259247f51222d955eb688519bb5886a4e904 ; _reflns_odcompleteness_completeness 99.51 _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, All C(H,H,H,H) groups 2. Restrained distances C59A-C53 = C59A-C60A 1.5 with sigma of 0.02 3. Rigid body (RIGU) restrains O51A, C53, C58, C59, C59A, C60A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(O51A)=Sof(H59C)=Sof(H59D)=Sof(C59A)=Sof(H59E)=Sof(H59F)=Sof(C60A)= Sof(H60C)=Sof(H60D)=1-FVAR(1) Sof(O51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)= Sof(H60B)=FVAR(1) Sof(O31A)=Sof(H32C)=Sof(H32D)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)= Sof(H40D)=1-FVAR(2) Sof(O31)=Sof(H32A)=Sof(H32B)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)= FVAR(2) 5.a Secondary CH2 refined with riding coordinates: C32(H32C,H32D), C32(H32A,H32B), C39(H39A,H39B), C39(H39C,H39D), C40(H40A, H40B), C40A(H40C,H40D), C52(H52A,H52B), C59(H59A,H59B), C59(H59C,H59D), C59A(H59E,H59F), C60(H60A,H60B), C60A(H60C,H60D) 5.b Aromatic/amide H refined with riding coordinates: C34(H34), C35(H35), C36(H36), C37(H37), C54(H54), C55(H55), C56(H56), C57(H57) ; _shelx_res_file ; TITL ohd494_8_numabs_ana2_a.res in P-1 REM Old TITL OHD494_8_numabs_ana2 in P-1 REM SHELXT solution in P-1 REM R1 0.167, Rweak 0.017, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C26 O2 F6 Ag CELL 1.54184 7.2534 11.0121 13.8225 85.841 85.713 84.263 ZERR 1 0.0003 0.0005 0.0006 0.004 0.003 0.003 LATT 1 SFAC C H Ag F O UNIT 50 40 2 10 8 DFIX 1.5 C59A C53 C59A C60A RIGU O51A C53 C58 C59 C59A C60A L.S. 4 0 0 PLAN 20 SIZE 0.028 0.032 0.11 TEMP -153.15 list 4 fmap 2 53 ACTA SHEL 50 0.8 REM REM REM WGHT 0.022300 1.887100 FVAR 0.58034 0.75240 0.68969 AG1 3 0.860021 0.422540 0.033967 11.00000 0.03237 0.04601 = 0.02840 -0.01641 0.00691 -0.01568 F20 4 0.877988 0.486672 0.350056 11.00000 0.05369 0.02348 = 0.02901 -0.00288 0.00197 -0.01315 F21 4 0.830689 0.593219 0.520191 11.00000 0.05257 0.03571 = 0.02144 0.00020 0.00494 -0.00799 F22 4 0.867579 0.834371 0.526017 11.00000 0.04612 0.03839 = 0.02490 -0.01450 0.00036 -0.00219 F23 4 0.949363 0.970963 0.359289 11.00000 0.04749 0.02219 = 0.03895 -0.00822 -0.00176 -0.00737 F24 4 1.002606 0.866152 0.188675 11.00000 0.03995 0.02811 = 0.02816 -0.00006 0.00220 -0.01153 O11 5 0.847508 0.547718 0.150979 11.00000 0.03301 0.03379 = 0.02637 -0.01233 0.00343 -0.01359 O13 5 1.116732 0.632548 0.116531 11.00000 0.02534 0.03291 = 0.02415 -0.00659 0.00232 -0.00721 PART 1 O31 5 0.565073 0.339959 0.107548 31.00000 0.02724 0.03555 = 0.03236 -0.00657 0.00509 -0.01331 PART 0 PART 2 O31A 5 0.541539 0.383393 0.097813 -31.00000 0.05358 0.04464 = 0.02590 -0.00744 0.00869 -0.03327 PART 0 C12 1 0.973142 0.611995 0.168089 11.00000 0.02754 0.02457 = 0.01979 -0.00369 -0.00101 -0.00517 C14 1 0.945624 0.672417 0.263753 11.00000 0.02200 0.02505 = 0.02298 -0.00633 0.00059 -0.00516 C15 1 0.898100 0.606748 0.350049 11.00000 0.03005 0.02481 = 0.02286 -0.00600 -0.00126 -0.00779 C16 1 0.873536 0.659886 0.437466 11.00000 0.02953 0.02922 = 0.02202 0.00015 -0.00010 -0.00543 C17 1 0.892243 0.782669 0.440947 11.00000 0.02585 0.03291 = 0.02422 -0.01021 -0.00119 -0.00213 C18 1 0.935840 0.850814 0.356374 11.00000 0.02584 0.02184 = 0.03178 -0.00756 -0.00166 -0.00414 C19 1 0.962753 0.796297 0.269654 11.00000 0.02375 0.02819 = 0.02626 -0.00020 -0.00010 -0.00833 C32 1 0.449194 0.305913 0.042069 11.00000 0.03615 0.04451 = 0.03104 -0.00587 0.00385 -0.01545 PART 2 AFIX 23 H32C 2 0.536261 0.233429 0.027487 -31.00000 -1.20000 H32D 2 0.421977 0.350800 -0.020706 -31.00000 -1.20000 AFIX 23 PART 0 PART 1 H32A 2 0.516193 0.239945 0.004491 31.00000 -1.20000 H32B 2 0.418598 0.376639 -0.004249 31.00000 -1.20000 AFIX 0 PART 0 C33 1 0.271075 0.261932 0.088361 11.00000 0.02696 0.02705 = 0.03183 0.00628 -0.00354 -0.00637 C34 1 0.161726 0.199309 0.033731 11.00000 0.03145 0.04028 = 0.03570 0.00507 -0.00679 -0.00896 AFIX 43 H34 2 0.200335 0.185316 -0.032048 11.00000 -1.20000 AFIX 0 C35 1 -0.002107 0.157432 0.074276 11.00000 0.03674 0.03496 = 0.05053 0.01022 -0.01677 -0.01061 AFIX 43 H35 2 -0.076549 0.115862 0.036348 11.00000 -1.20000 AFIX 0 C36 1 -0.056850 0.176444 0.170334 11.00000 0.02452 0.03849 = 0.05655 0.01373 -0.00225 -0.00877 AFIX 43 H36 2 -0.168362 0.146874 0.198909 11.00000 -1.20000 AFIX 0 C37 1 0.050433 0.238390 0.224798 11.00000 0.03360 0.04329 = 0.04297 0.00142 0.00617 -0.00950 AFIX 43 H37 2 0.011741 0.251231 0.290757 11.00000 -1.20000 AFIX 0 C38 1 0.215323 0.282526 0.184246 11.00000 0.02633 0.02398 = 0.03343 0.00266 0.00238 -0.00269 C39 1 0.333239 0.350553 0.243150 11.00000 0.03684 0.04050 = 0.03005 -0.00779 0.00716 -0.01275 PART 1 AFIX 23 H39A 2 0.252154 0.410926 0.280460 31.00000 -1.20000 H39B 2 0.397461 0.292018 0.290210 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H39C 2 0.276914 0.435867 0.247179 -31.00000 -1.20000 H39D 2 0.333882 0.311887 0.310071 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C40 1 0.474160 0.415246 0.180307 31.00000 0.03495 0.03597 = 0.03593 -0.01000 0.00352 -0.01269 AFIX 23 H40A 2 0.412369 0.490211 0.148361 31.00000 -1.20000 H40B 2 0.568049 0.440232 0.221402 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C40A 1 0.524460 0.351830 0.201952 -31.00000 0.03330 0.04388 = 0.02641 -0.01165 0.01041 -0.01685 AFIX 23 H40C 2 0.586521 0.411251 0.235509 -31.00000 -1.20000 H40D 2 0.590858 0.269975 0.215119 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 O51 5 0.566851 0.860886 0.173187 21.00000 0.03376 0.04799 = 0.03208 0.00112 0.00012 -0.00634 PART 0 PART 2 O51A 5 0.538887 1.012329 0.220434 -21.00000 0.03993 0.02932 = 0.04134 -0.00098 -0.00453 -0.01222 PART 0 PART 1 C52 1 0.482242 0.755664 0.214284 21.00000 0.03146 0.03714 = 0.03834 -0.01321 0.00015 -0.00518 AFIX 23 H52A 2 0.568843 0.681301 0.205491 21.00000 -1.20000 H52B 2 0.368451 0.746851 0.181101 21.00000 -1.20000 AFIX 0 PART 0 C53 1 0.434212 0.770004 0.320423 11.00000 0.02085 0.04695 = 0.03607 -0.01471 -0.00159 -0.00828 C54 1 0.410488 0.662736 0.378528 11.00000 0.03306 0.03098 = 0.05984 -0.01923 0.00018 -0.00823 AFIX 43 H54 2 0.425169 0.586568 0.349336 11.00000 -1.20000 AFIX 0 C55 1 0.366635 0.664727 0.476428 11.00000 0.03542 0.03179 = 0.05654 0.00410 -0.00537 -0.00994 AFIX 43 H55 2 0.352757 0.590611 0.514741 11.00000 -1.20000 AFIX 0 C56 1 0.342855 0.774460 0.518855 11.00000 0.03298 0.04375 = 0.03217 -0.00132 -0.00048 -0.00917 AFIX 43 H56 2 0.309810 0.776724 0.586559 11.00000 -1.20000 AFIX 0 C57 1 0.366961 0.881735 0.463128 11.00000 0.03102 0.03002 = 0.03873 -0.00936 -0.00276 -0.00384 AFIX 43 H57 2 0.351010 0.957299 0.493213 11.00000 -1.20000 AFIX 0 C58 1 0.414084 0.881070 0.363936 11.00000 0.02476 0.03278 = 0.03198 -0.00320 -0.00287 -0.00527 C59 1 0.445743 0.997747 0.303958 11.00000 0.04059 0.04482 = 0.04717 0.00968 -0.00480 -0.01120 PART 1 AFIX 23 H59A 2 0.564042 1.027372 0.319205 21.00000 -1.20000 H59B 2 0.343657 1.061628 0.318938 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H59C 2 0.319945 1.038285 0.293824 -21.00000 -1.20000 H59D 2 0.501620 1.048893 0.347773 -21.00000 -1.20000 AFIX 0 C59A 1 0.467752 0.802477 0.208610 -21.00000 0.01884 0.02761 = 0.04038 -0.01666 0.00092 -0.00722 AFIX 23 H59E 2 0.594343 0.766049 0.189369 -21.00000 -1.20000 H59F 2 0.380667 0.757888 0.175990 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C60 1 0.453067 0.971432 0.193838 21.00000 0.04083 0.03178 = 0.05233 0.01345 -0.00157 -0.00289 AFIX 23 H60A 2 0.325505 0.964845 0.175135 21.00000 -1.20000 H60B 2 0.502755 1.040884 0.154178 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C60A 1 0.452094 0.932709 0.163480 -21.00000 0.03035 0.03146 = 0.04682 -0.00427 0.00131 -0.00927 AFIX 23 H60C 2 0.512259 0.934086 0.096769 -21.00000 -1.20000 H60D 2 0.319435 0.962523 0.159070 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ohd494_8_numabs_ana2_a.res in P-1 REM R1 = 0.0355 for 3829 Fo > 4sig(Fo) and 0.0445 for all 4439 data REM 363 parameters refined using 38 restraints END WGHT 0.0223 1.8870 REM Highest difference peak 1.533, deepest hole -1.435, 1-sigma level 0.085 Q1 1 0.7986 0.4780 0.0072 11.00000 0.05 1.53 Q2 1 0.8427 0.4265 0.0838 11.00000 0.05 0.60 Q3 1 0.7726 0.5172 0.0805 11.00000 0.05 0.43 Q4 1 0.5065 0.2965 -0.0208 11.00000 0.05 0.42 Q5 1 0.9576 0.6403 0.2190 11.00000 0.05 0.40 Q6 1 0.8621 0.4538 -0.0571 11.00000 0.05 0.40 Q7 1 0.8929 0.3570 0.1256 11.00000 0.05 0.38 Q8 1 0.3588 0.2842 0.0639 11.00000 0.05 0.35 Q9 1 0.8195 0.3790 0.0354 11.00000 0.05 0.32 Q10 1 0.0817 0.1781 0.0549 11.00000 0.05 0.32 Q11 1 0.7513 0.4031 -0.0415 11.00000 0.05 0.32 Q12 1 0.9732 0.4567 0.0975 11.00000 0.05 0.32 Q13 1 0.5951 0.1854 0.0559 11.00000 0.05 0.31 Q14 1 0.4771 0.7777 0.2641 11.00000 0.05 0.31 Q15 1 1.0211 0.3780 0.0767 11.00000 0.05 0.31 Q16 1 0.9383 0.3004 0.0268 11.00000 0.05 0.30 Q17 1 0.2762 0.3553 0.2978 11.00000 0.05 0.30 Q18 1 0.9545 0.3214 0.0076 11.00000 0.05 0.29 Q19 1 0.6780 0.8811 0.4401 11.00000 0.05 0.28 Q20 1 0.9413 0.4253 0.1219 11.00000 0.05 0.28 ; _shelx_res_checksum 51604 _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 1.577 _oxdiff_exptl_absorpt_empirical_full_min 0.605 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 0.86002(4) 0.42254(3) 0.03397(2) 0.03455(9) Uani 1 1 d . . . . . F20 F 0.8780(3) 0.48667(16) 0.35006(14) 0.0349(5) Uani 1 1 d . . . . . F21 F 0.8307(3) 0.59322(18) 0.52019(14) 0.0368(5) Uani 1 1 d . . . . . F22 F 0.8676(3) 0.83437(18) 0.52602(14) 0.0361(5) Uani 1 1 d . . . . . F23 F 0.9494(3) 0.97096(16) 0.35929(15) 0.0357(5) Uani 1 1 d . . . . . F24 F 1.0026(3) 0.86615(17) 0.18867(13) 0.0318(4) Uani 1 1 d . . . . . O11 O 0.8475(3) 0.5477(2) 0.15098(16) 0.0301(5) Uani 1 1 d . . . . . O13 O 1.1167(3) 0.6325(2) 0.11653(16) 0.0271(5) Uani 1 1 d . . . . . O31 O 0.5651(15) 0.3400(8) 0.1075(9) 0.0312(17) Uani 0.69(2) 1 d . . P A 1 O31A O 0.542(4) 0.383(2) 0.0978(19) 0.040(5) Uani 0.31(2) 1 d . . P A 2 C12 C 0.9731(4) 0.6120(3) 0.1681(2) 0.0237(6) Uani 1 1 d . . . . . C14 C 0.9456(4) 0.6724(3) 0.2638(2) 0.0230(6) Uani 1 1 d . . . . . C15 C 0.8981(5) 0.6067(3) 0.3500(2) 0.0254(7) Uani 1 1 d . . . . . C16 C 0.8735(5) 0.6599(3) 0.4375(2) 0.0269(7) Uani 1 1 d . . . . . C17 C 0.8922(5) 0.7827(3) 0.4409(2) 0.0273(7) Uani 1 1 d . . . . . C18 C 0.9358(5) 0.8508(3) 0.3564(2) 0.0261(7) Uani 1 1 d . . . . . C19 C 0.9628(4) 0.7963(3) 0.2697(2) 0.0258(7) Uani 1 1 d . . . . . C32 C 0.4492(5) 0.3059(4) 0.0421(3) 0.0366(8) Uani 1 1 d . . . . . H32C H 0.5363 0.2334 0.0275 0.044 Uiso 0.31(2) 1 calc R . P A 2 H32D H 0.4220 0.3508 -0.0207 0.044 Uiso 0.31(2) 1 calc R . P A 2 H32A H 0.5162 0.2399 0.0045 0.044 Uiso 0.69(2) 1 calc R . P A 1 H32B H 0.4186 0.3766 -0.0042 0.044 Uiso 0.69(2) 1 calc R . P A 1 C33 C 0.2711(5) 0.2619(3) 0.0884(2) 0.0287(7) Uani 1 1 d . . . . . C34 C 0.1617(5) 0.1993(3) 0.0337(3) 0.0356(8) Uani 1 1 d . . . . . H34 H 0.2003 0.1853 -0.0320 0.043 Uiso 1 1 calc R . . . . C35 C -0.0021(5) 0.1574(3) 0.0743(3) 0.0402(9) Uani 1 1 d . . . . . H35 H -0.0765 0.1159 0.0363 0.048 Uiso 1 1 calc R . . . . C36 C -0.0568(5) 0.1764(3) 0.1703(3) 0.0403(9) Uani 1 1 d . . . . . H36 H -0.1684 0.1469 0.1989 0.048 Uiso 1 1 calc R . . . . C37 C 0.0504(5) 0.2384(4) 0.2248(3) 0.0402(9) Uani 1 1 d . . . . . H37 H 0.0117 0.2512 0.2908 0.048 Uiso 1 1 calc R . . . . C38 C 0.2153(5) 0.2825(3) 0.1842(3) 0.0283(7) Uani 1 1 d . . . . . C39 C 0.3332(5) 0.3506(3) 0.2431(3) 0.0354(8) Uani 1 1 d . . . . . H39A H 0.2522 0.4109 0.2805 0.042 Uiso 0.69(2) 1 calc R . P A 1 H39B H 0.3975 0.2920 0.2902 0.042 Uiso 0.69(2) 1 calc R . P A 1 H39C H 0.2769 0.4359 0.2472 0.042 Uiso 0.31(2) 1 calc R . P A 2 H39D H 0.3339 0.3119 0.3101 0.042 Uiso 0.31(2) 1 calc R . P A 2 C40 C 0.4742(11) 0.4152(10) 0.1803(6) 0.035(2) Uani 0.69(2) 1 d . . P A 1 H40A H 0.4124 0.4902 0.1484 0.042 Uiso 0.69(2) 1 calc R . P A 1 H40B H 0.5680 0.4402 0.2214 0.042 Uiso 0.69(2) 1 calc R . P A 1 C40A C 0.524(2) 0.352(2) 0.2020(11) 0.034(5) Uani 0.31(2) 1 d . . P A 2 H40C H 0.5865 0.4113 0.2355 0.041 Uiso 0.31(2) 1 calc R . P A 2 H40D H 0.5909 0.2700 0.2151 0.041 Uiso 0.31(2) 1 calc R . P A 2 O51 O 0.5669(5) 0.8609(3) 0.1732(2) 0.0381(12) Uani 0.752(8) 1 d . . P B 1 O51A O 0.5389(17) 1.0123(10) 0.2204(8) 0.036(3) Uani 0.248(8) 1 d . U P B 2 C52 C 0.4822(11) 0.7557(6) 0.2143(5) 0.0351(15) Uani 0.752(8) 1 d . . P B 1 H52A H 0.5688 0.6813 0.2055 0.042 Uiso 0.752(8) 1 calc R . P B 1 H52B H 0.3685 0.7469 0.1811 0.042 Uiso 0.752(8) 1 calc R . P B 1 C53 C 0.4342(5) 0.7700(3) 0.3204(3) 0.0337(8) Uani 1 1 d D U . . . C54 C 0.4105(5) 0.6627(3) 0.3785(3) 0.0403(9) Uani 1 1 d . . . . . H54 H 0.4252 0.5866 0.3493 0.048 Uiso 1 1 calc R . . . . C55 C 0.3666(5) 0.6647(3) 0.4764(3) 0.0410(9) Uani 1 1 d . . . . . H55 H 0.3528 0.5906 0.5147 0.049 Uiso 1 1 calc R . . . . C56 C 0.3429(5) 0.7745(3) 0.5189(3) 0.0361(8) Uani 1 1 d . . . . . H56 H 0.3098 0.7767 0.5866 0.043 Uiso 1 1 calc R . . . . C57 C 0.3670(5) 0.8817(3) 0.4631(3) 0.0328(8) Uani 1 1 d . . . . . H57 H 0.3510 0.9573 0.4932 0.039 Uiso 1 1 calc R . . . . C58 C 0.4141(5) 0.8811(3) 0.3639(3) 0.0296(7) Uani 1 1 d . U . . . C59 C 0.4457(6) 0.9977(4) 0.3040(3) 0.0442(9) Uani 1 1 d . U . . . H59A H 0.5640 1.0274 0.3192 0.053 Uiso 0.752(8) 1 calc R . P B 1 H59B H 0.3437 1.0616 0.3189 0.053 Uiso 0.752(8) 1 calc R . P B 1 H59C H 0.3199 1.0383 0.2938 0.053 Uiso 0.248(8) 1 calc R . P B 2 H59D H 0.5016 1.0489 0.3478 0.053 Uiso 0.248(8) 1 calc R . P B 2 C59A C 0.468(3) 0.8025(15) 0.2086(12) 0.028(4) Uani 0.248(8) 1 d D U P B 2 H59E H 0.5943 0.7660 0.1894 0.034 Uiso 0.248(8) 1 calc R . P B 2 H59F H 0.3807 0.7579 0.1760 0.034 Uiso 0.248(8) 1 calc R . P B 2 C60 C 0.4531(11) 0.9714(6) 0.1938(5) 0.0426(18) Uani 0.752(8) 1 d . . P B 1 H60A H 0.3255 0.9648 0.1751 0.051 Uiso 0.752(8) 1 calc R . P B 1 H60B H 0.5028 1.0409 0.1542 0.051 Uiso 0.752(8) 1 calc R . P B 1 C60A C 0.452(3) 0.9327(16) 0.1635(16) 0.036(5) Uani 0.248(8) 1 d D U P B 2 H60C H 0.5123 0.9341 0.0968 0.043 Uiso 0.248(8) 1 calc R . P B 2 H60D H 0.3194 0.9625 0.1591 0.043 Uiso 0.248(8) 1 calc R . P B 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 0.03237(14) 0.04601(16) 0.02840(14) -0.01641(10) 0.00691(10) -0.01568(11) F20 0.0537(13) 0.0235(9) 0.0290(10) -0.0029(8) 0.0020(9) -0.0132(9) F21 0.0526(13) 0.0357(11) 0.0214(9) 0.0002(8) 0.0049(9) -0.0080(9) F22 0.0461(13) 0.0384(11) 0.0249(10) -0.0145(8) 0.0004(9) -0.0022(9) F23 0.0475(13) 0.0222(9) 0.0390(11) -0.0082(8) -0.0018(9) -0.0074(8) F24 0.0400(11) 0.0281(10) 0.0282(10) -0.0001(8) 0.0022(8) -0.0115(8) O11 0.0330(13) 0.0338(12) 0.0264(12) -0.0123(10) 0.0034(10) -0.0136(10) O13 0.0253(12) 0.0329(12) 0.0242(11) -0.0066(9) 0.0023(9) -0.0072(9) O31 0.027(2) 0.036(4) 0.032(3) -0.007(4) 0.005(2) -0.013(3) O31A 0.054(11) 0.045(11) 0.026(7) -0.007(9) 0.009(6) -0.033(10) C12 0.0275(17) 0.0246(15) 0.0198(15) -0.0037(12) -0.0010(13) -0.0052(13) C14 0.0220(16) 0.0250(15) 0.0230(15) -0.0063(13) 0.0006(12) -0.0052(12) C15 0.0301(17) 0.0248(15) 0.0229(16) -0.0060(13) -0.0013(13) -0.0078(13) C16 0.0295(17) 0.0292(17) 0.0220(16) 0.0001(13) -0.0001(13) -0.0054(13) C17 0.0258(17) 0.0329(17) 0.0242(16) -0.0102(14) -0.0012(13) -0.0021(13) C18 0.0258(17) 0.0218(15) 0.0318(17) -0.0076(13) -0.0017(13) -0.0041(12) C19 0.0238(16) 0.0282(16) 0.0263(16) -0.0002(13) -0.0001(13) -0.0083(13) C32 0.036(2) 0.045(2) 0.0310(19) -0.0059(16) 0.0038(15) -0.0155(16) C33 0.0270(17) 0.0271(16) 0.0318(18) 0.0063(14) -0.0035(14) -0.0064(13) C34 0.0315(19) 0.040(2) 0.0357(19) 0.0051(16) -0.0068(15) -0.0090(15) C35 0.037(2) 0.0350(19) 0.051(2) 0.0102(18) -0.0168(18) -0.0106(16) C36 0.0245(18) 0.038(2) 0.057(3) 0.0137(18) -0.0023(17) -0.0088(15) C37 0.034(2) 0.043(2) 0.043(2) 0.0014(17) 0.0062(17) -0.0095(16) C38 0.0263(17) 0.0240(16) 0.0334(18) 0.0027(14) 0.0024(14) -0.0027(13) C39 0.037(2) 0.040(2) 0.0301(18) -0.0078(15) 0.0072(15) -0.0127(16) C40 0.035(4) 0.036(5) 0.036(3) -0.010(3) 0.004(3) -0.013(3) C40A 0.033(8) 0.044(11) 0.026(7) -0.012(7) 0.010(6) -0.017(7) O51 0.034(2) 0.048(2) 0.0321(19) 0.0011(16) 0.0001(15) -0.0063(18) O51A 0.040(6) 0.029(5) 0.041(5) -0.001(4) -0.005(4) -0.012(4) C52 0.031(3) 0.037(4) 0.038(3) -0.013(3) 0.000(2) -0.005(3) C53 0.0208(17) 0.047(2) 0.0361(19) -0.0147(16) -0.0016(14) -0.0083(14) C54 0.033(2) 0.0310(18) 0.060(3) -0.0192(18) 0.0002(18) -0.0082(15) C55 0.035(2) 0.0318(19) 0.057(3) 0.0041(18) -0.0054(18) -0.0099(16) C56 0.0330(19) 0.044(2) 0.0322(19) -0.0013(16) -0.0005(15) -0.0092(16) C57 0.0310(19) 0.0300(17) 0.0387(19) -0.0094(15) -0.0028(15) -0.0038(14) C58 0.0248(17) 0.0328(17) 0.0320(17) -0.0032(14) -0.0029(14) -0.0053(13) C59 0.041(2) 0.045(2) 0.047(2) 0.0097(18) -0.0048(18) -0.0112(17) C59A 0.019(8) 0.028(7) 0.040(5) -0.017(4) 0.001(5) -0.007(7) C60 0.041(4) 0.032(4) 0.052(4) 0.013(3) -0.002(3) -0.003(3) C60A 0.030(9) 0.031(7) 0.047(7) -0.004(5) 0.001(6) -0.009(6) 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 -6 -5 0.0171 0 6 5 0.0111 5 0 0 0.0584 -5 0 0 0.0424 0 7 -3 0.0161 0 1 -9 0.0138 0 -5 6 0.0093 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 78.23(6) . 2_765 ? O11 Ag1 O13 156.93(8) . 2_765 ? O11 Ag1 O31 89.7(3) . . ? O11 Ag1 O31A 84.9(6) . . ? O13 Ag1 Ag1 84.29(6) 2_765 2_765 ? O13 Ag1 O31 104.3(3) 2_765 . ? O13 Ag1 O31A 105.3(6) 2_765 . ? O31 Ag1 Ag1 164.2(2) . 2_765 ? O31A Ag1 Ag1 153.4(6) . 2_765 ? C12 O11 Ag1 125.9(2) . . ? C12 O13 Ag1 118.0(2) . 2_765 ? C32 O31 Ag1 115.4(7) . . ? C32 O31 C40 114.4(8) . . ? C40 O31 Ag1 111.9(7) . . ? C32 O31A Ag1 115.3(15) . . ? C32 O31A C40A 113.4(17) . . ? C40A O31A Ag1 114.0(18) . . ? O11 C12 C14 115.4(3) . . ? O13 C12 O11 128.4(3) . . ? O13 C12 C14 116.2(3) . . ? C15 C14 C12 121.3(3) . . ? C15 C14 C19 116.6(3) . . ? C19 C14 C12 122.1(3) . . ? F20 C15 C14 120.1(3) . . ? F20 C15 C16 117.8(3) . . ? C16 C15 C14 122.1(3) . . ? F21 C16 C15 120.7(3) . . ? F21 C16 C17 119.4(3) . . ? C15 C16 C17 119.9(3) . . ? F22 C17 C16 119.8(3) . . ? F22 C17 C18 120.8(3) . . ? C18 C17 C16 119.4(3) . . ? F23 C18 C17 119.5(3) . . ? F23 C18 C19 120.3(3) . . ? C19 C18 C17 120.2(3) . . ? F24 C19 C14 119.8(3) . . ? F24 C19 C18 118.3(3) . . ? C18 C19 C14 121.8(3) . . ? O31 C32 C33 113.9(6) . . ? O31A C32 C33 116.3(11) . . ? C34 C33 C32 119.4(3) . . ? C38 C33 C32 120.8(3) . . ? C38 C33 C34 119.8(3) . . ? C35 C34 C33 120.7(4) . . ? C36 C35 C34 119.6(4) . . ? C37 C36 C35 120.0(3) . . ? C36 C37 C38 120.9(4) . . ? C33 C38 C37 118.9(3) . . ? C33 C38 C39 119.8(3) . . ? C37 C38 C39 121.3(3) . . ? C40 C39 C38 111.9(4) . . ? C40A C39 C38 112.9(6) . . ? O31 C40 C39 112.0(9) . . ? O31A C40A C39 114(2) . . ? C52 O51 C60 111.3(5) . . ? C59 O51A C60A 100.8(11) . . ? O51 C52 C53 109.0(5) . . ? C54 C53 C52 116.5(4) . . ? C54 C53 C59A 135.2(7) . . ? C58 C53 C52 124.7(4) . . ? C58 C53 C54 118.8(3) . . ? C58 C53 C59A 105.9(7) . . ? C55 C54 C53 121.6(3) . . ? C54 C55 C56 119.5(3) . . ? C55 C56 C57 120.0(4) . . ? C56 C57 C58 121.2(3) . . ? C53 C58 C59 120.1(3) . . ? C57 C58 C53 118.9(3) . . ? C57 C58 C59 121.0(3) . . ? O51A C59 C58 128.9(6) . . ? C58 C59 C60 108.5(4) . . ? C60A C59A C53 123.2(14) . . ? O51 C60 C59 112.1(4) . . ? O51A C60A C59A 111.0(17) . . ? 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 2.8444(5) 2_765 ? Ag1 O11 2.191(2) . ? Ag1 O13 2.199(2) 2_765 ? Ag1 O31 2.523(11) . ? Ag1 O31A 2.48(3) . ? F20 C15 1.345(3) . ? F21 C16 1.347(4) . ? F22 C17 1.336(4) . ? F23 C18 1.340(3) . ? F24 C19 1.341(3) . ? O11 C12 1.254(4) . ? O13 Ag1 2.199(2) 2_765 ? O13 C12 1.248(4) . ? O31 C32 1.376(12) . ? O31 C40 1.430(14) . ? O31A C32 1.43(3) . ? O31A C40A 1.46(3) . ? C12 C14 1.514(4) . ? C14 C15 1.388(4) . ? C14 C19 1.391(4) . ? C15 C16 1.372(5) . ? C16 C17 1.377(5) . ? C17 C18 1.376(5) . ? C18 C19 1.372(5) . ? C32 C33 1.507(5) . ? C33 C34 1.396(5) . ? C33 C38 1.384(5) . ? C34 C35 1.383(5) . ? C35 C36 1.382(6) . ? C36 C37 1.381(6) . ? C37 C38 1.399(5) . ? C38 C39 1.509(5) . ? C39 C40 1.493(8) . ? C39 C40A 1.460(14) . ? O51 C52 1.427(7) . ? O51 C60 1.435(8) . ? O51A C59 1.301(11) . ? O51A C60A 1.44(2) . ? C52 C53 1.498(7) . ? C53 C54 1.397(5) . ? C53 C58 1.392(5) . ? C53 C59A 1.567(16) . ? C54 C55 1.368(6) . ? C55 C56 1.371(5) . ? C56 C57 1.382(5) . ? C57 C58 1.388(5) . ? C58 C59 1.506(5) . ? C59 C60 1.566(9) . ? C59A C60A 1.519(17) . ? 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 0.0043 -5.9571 -5.3670 0.0248 0.9987 0.0435 -0.0043 5.9571 5.3670 -0.0248 -0.9987 -0.0435 4.6117 -0.4973 -0.4305 -0.8585 0.2034 0.4708 -4.6117 0.4973 0.4305 0.8585 -0.2034 -0.4708 0.3310 6.5367 -3.0256 -0.4706 -0.5006 -0.7266 0.3601 1.0909 -8.6695 -0.4841 0.4616 -0.7433 0.0025 -4.9603 6.0543 0.4702 0.1393 0.8775