The atypical solubility of silver(i) pentafluorobenzoate and its use as a catch-and-release agent
Ward, Jas S.; CrystEngComm 26 (2024) 3088–3097; doi:10.1039/D4CE00441H

data_7248652
_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         'C11 H10 Ag F5 O3'
_chemical_formula_sum            'C11 H10 Ag F5 O3'
_chemical_formula_weight         393.06
_chemical_properties_physical    'Desolvates rapidly.'
_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             2023-10-13
_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                82.824(3)
_cell_angle_beta                 80.970(3)
_cell_angle_gamma                75.189(3)
_cell_formula_units_Z            2
_cell_length_a                   5.4941(2)
_cell_length_b                   9.8998(3)
_cell_length_c                   12.7267(5)
_cell_measurement_reflns_used    7104
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.1980
_cell_measurement_theta_min      4.6230
_cell_volume                     658.31(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_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.951
_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    0.50    --  -87.61  57.00 150.00   82
  2  \w    -54.00 -13.00   0.50    0.50    --  -87.61  57.00  60.00   82
  3  \w   -112.00 -20.00   0.50    0.50    --  -87.61  77.00  90.00  184
  4  \w   -112.00 -20.00   0.50    0.50    --  -87.61  77.00 -60.00  184
  5  \w    -54.00 -13.00   0.50    0.50    --  -87.61  57.00 -30.00   82
  6  \w    -27.00  26.00   0.50    0.15    --  -51.51  38.00 -90.00  106
  7  \w     16.00  42.00   0.50    0.15    --   46.00  87.00  29.23   52
  8  \w    -35.00  -4.00   0.50    0.15    --   10.00 113.00 -17.94   62
  9  \w     15.00  42.00   0.50    0.15    --   46.00  89.00-110.02   54
 10  \w     80.00 173.00   0.50    0.50    --  102.08 125.00  30.00  186
 11  \w     78.00 169.00   0.50    0.50    --  102.08  77.00-120.00  182
 12  \w     88.00 176.00   0.50    0.50    --  102.08  38.00 -60.00  176
 13  \w     85.00 176.00   0.50    0.50    --  102.08  57.00 -60.00  182
 14  \w     88.00 176.00   0.50    0.50    --  102.08  38.00  30.00  176
 15  \w     36.00 176.00   0.50    0.50    --  102.08   7.00 -94.00  280
 16  \w     16.00 126.00   0.50    0.15    --   51.89   7.00 -94.00  220
 17  \w     78.00 169.00   0.50    0.50    --  102.08  77.00-150.00  182
 18  \w     28.00  79.00   0.50    0.50    --  102.08 -57.00-150.00  102
 19  \w     28.00  79.00   0.50    0.50    --  102.08 -57.00-120.00  102
 20  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00 -90.00   54
 21  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00 -60.00   54
 22  \w     28.00  79.00   0.50    0.50    --  102.08 -57.00   0.00  102
 23  \w     28.00  79.00   0.50    0.50    --  102.08 -57.00  30.00  102
 24  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00  90.00   54
 25  \w     28.00  79.00   0.50    0.50    --  102.08 -57.00 120.00  102
 26  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00   0.00   54
 27  \w    -22.00   9.00   0.50    0.15    --   51.89  -7.00  89.00   62
 28  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00 -30.00   54
 29  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00-180.00   54
 30  \w     25.00  52.00   0.50    0.50    --  102.08 -38.00-150.00   54
 31  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00 -30.00  142
 32  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00-120.00  142
 33  \w     32.00 111.00   0.50    0.50    --  102.08-125.00-120.00  158
 34  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00   0.00  142
 35  \w     32.00 111.00   0.50    0.50    --  102.08-125.00   0.00  158
 36  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00  30.00  142
 37  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00  60.00  142
 38  \w     35.00 106.00   0.50    0.50    --  102.08 -99.00 150.00  142
 39  \w     32.00 111.00   0.50    0.50    --  102.08-125.00 150.00  158
 40  \w   -119.00 -27.00   0.50    0.15    --  -51.51 -77.00  90.00  184
 41  \w   -159.00 -68.00   0.50    0.50    --  -90.00 -73.00 110.74  182
 42  \w   -155.00 -63.00   0.50    0.50    --  -87.61 -77.00  90.00  184
 43  \w   -136.00 -46.00   0.50    0.15    --  -66.00 -70.00  39.82  180
 44  \w   -138.00 -46.00   0.50    0.15    --  -70.00 -76.00 -16.78  184
 45  \w   -160.00 -70.00   0.50    0.50    --  -90.00 -70.00 -44.83  180
 46  \w   -147.00 -56.00   0.50    0.15    --  -78.00 -73.00-152.55  182
 47  \w   -149.00 -58.00   0.50    0.15    --  -78.00 -68.00 -73.78  182
 48  \w   -165.00 -75.00   0.50    0.50    --  -95.50 -71.00 -13.07  180
 49  \w   -149.00 -58.00   0.50    0.15    --  -78.00 -68.00 -99.31  182
 50  \w   -167.00 -76.00   0.50    0.50    --  -95.50 -67.00  61.56  182
 51  \w   -159.00 -67.00   0.50    0.50    --  -86.00 -62.00  15.34  184
 52  \w   -167.00 -76.00   0.50    0.50    --  -95.50 -66.00 125.47  182
 53  \w   -166.00 -75.00   0.50    0.50    --  -95.50 -69.00 146.90  182
 54  \w   -152.00 -62.00   0.50    0.50    --  -82.00 -69.00 177.34  180
 55  \w   -166.00 -75.00   0.50    0.50    --  -95.50 -68.00 161.37  182
 56  \w   -125.00   9.00   0.50    0.15    --  -51.51  -7.00  89.00  268
 57  \w   -159.00 -21.00   0.50    0.50    --  -87.61  -7.00  89.00  276
;
_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      0.2875513000
_diffrn_orient_matrix_UB_12      -0.0109498000
_diffrn_orient_matrix_UB_13      -0.0113025000
_diffrn_orient_matrix_UB_21      0.0523718000
_diffrn_orient_matrix_UB_22      -0.1606017000
_diffrn_orient_matrix_UB_23      0.0009153000
_diffrn_orient_matrix_UB_31      0.0121570000
_diffrn_orient_matrix_UB_32      0.0142229000
_diffrn_orient_matrix_UB_33      -0.1225311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19770
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_min         5.578
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.942
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2554
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+0.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2411
_reflns_number_total             2554
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 1.8960\% 
around [0.74 0.64 0.21] (reciprocal) or [0.99 0.14 -0.03] (direct)
;
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_Et2O
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248652
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C22 H20 Ag2 F10 O6'
_chemical_oxdiff_usercomment     'Et2O evap'
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.247
_diffrn_oxdiff_digest_frames
;
01570d1618165e7bf2173bac8d803a50330820405b2
;
_diffrn_oxdiff_digest_hkl
;
018dba80ddf7381c45bebddd58e2b62e4b24b5
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C35 = C38-C39
 1.5 with sigma of 0.02
 O31-C38 = O31-C36
 1.4 with sigma of 0.02
 O31-C32
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O31 \\sim C32 \\sim C33 \\sim C34 \\sim C36 \\sim C37 \\sim C38 \\sim C39:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C34) = Uanis(C35)
4. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B)
5.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C)
;
_shelx_res_checksum              72972
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.734
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2