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_7248663
_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         '2(C21 H8 Ag2 F10 O4)'
_chemical_formula_sum            'C42 H16 Ag4 F20 O8'
_chemical_formula_weight         1460.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.194(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.60970(10)
_cell_length_b                   55.4509(15)
_cell_length_c                   13.6451(4)
_cell_measurement_reflns_used    12622
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6640
_cell_measurement_theta_min      3.6180
_cell_volume                     4211.07(18)
_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 0.996
_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     57.00 113.00   0.50    0.50    --   42.17 161.00 -65.00  112
  2  \w     -3.00  22.00   0.50    0.50    --   46.00 100.00  35.28   50
  3  \w      2.00  28.00   0.50    0.50    --   50.00  96.00 -34.58   52
  4  \w      4.00  41.00   0.50    0.50    --   46.00  86.00 -58.16   74
  5  \w     12.00  42.00   0.50    0.50    --   50.00  82.00-121.76   60
  6  \w     15.00  40.00   0.50    0.50    --   58.00  88.00-146.41   50
  7  \w     87.00 157.00   0.50    1.20    --  113.05  45.00-180.00  140
  8  \w    104.00 130.00   0.50    1.20    --  113.05 161.00 -65.00   52
  9  \w    113.00 139.00   0.50    1.20    --  113.05 118.00 142.00   52
 10  \w    112.00 175.00   0.50    1.20    --  113.05  45.00  60.00  126
 11  \w     87.00 171.00   0.50    1.20    --  113.05  45.00  30.00  168
 12  \w     28.00  53.00   0.50    1.20    --  113.05 -45.00 -90.00   50
 13  \w     36.00  61.00   0.50    1.20    --  113.05 -45.00-120.00   50
 14  \w     86.00 111.00   0.50    1.20    --  113.05-125.00-180.00   50
 15  \w     64.00  89.00   0.50    1.20    --  113.05-161.00 -95.00   50
 16  \w     39.00 110.00   0.50    1.20    --  113.05-125.00 -90.00  142
 17  \w     38.00 129.00   0.50    0.50    --   42.17-161.00 -95.00  182
 18  \w     63.00 106.00   0.50    1.20    --  113.05-118.00  56.00   86
 19  \w     32.00 104.00   0.50    1.20    --  113.05 -95.00  60.00  144
 20  \w     40.00  81.00   0.50    1.20    --  113.05 -95.00  90.00   82
 21  \w     33.00  59.00   0.50    1.20    --  113.05 -45.00  60.00   52
 22  \w     33.00  99.00   0.50    1.20    --  113.05 -95.00 -90.00  132
 23  \w     15.00 102.00   0.50    0.50    --   42.17-118.00  56.00  174
 24  \w   -101.00 -75.00   0.50    1.20    --  -89.35 118.00 142.00   52
 25  \w    -59.00 -20.00   0.50    1.20    --  -89.35  61.00 120.00   78
 26  \w    -60.00 -31.00   0.50    1.20    --  -89.35  61.00  90.00   58
 27  \w    -37.00  -5.00   0.50    1.20    --  -89.35  45.00 -30.00   64
 28  \w    -37.00 -12.00   0.50    1.20    --  -89.35  45.00 -60.00   50
 29  \w   -135.00 -38.00   0.50    1.20    --  -89.35 161.00 -65.00  194
 30  \w   -130.00 -31.00   0.50    0.50    --  -41.73 161.00 -65.00  198
 31  \w    -37.00  -6.00   0.50    1.20    --  -89.35  45.00-120.00   62
 32  \w    -37.00  -9.00   0.50    1.20    --  -89.35  45.00 -90.00   56
 33  \w    -33.00  -5.00   0.50    1.20    --  -89.35  45.00   0.00   56
 34  \w   -149.00 -38.00   0.50    0.50    --  -70.00 -63.00  74.20  222
 35  \w   -129.00 -92.00   0.50    1.20    --  -89.35-118.00  56.00   74
 36  \w   -124.00 -54.00   0.50    0.50    --  -41.73-178.00  60.00  140
 37  \w   -156.00 -50.00   0.50    1.20    --  -89.35-161.00 -95.00  212
 38  \w   -113.00 -51.00   0.50    0.50    --  -41.73-161.00 -95.00  124
;
_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      -0.1395552000
_diffrn_orient_matrix_UB_12      0.0043321000
_diffrn_orient_matrix_UB_13      0.0887180000
_diffrn_orient_matrix_UB_21      0.0137664000
_diffrn_orient_matrix_UB_22      -0.0271164000
_diffrn_orient_matrix_UB_23      0.0243698000
_diffrn_orient_matrix_UB_31      0.2386614000
_diffrn_orient_matrix_UB_32      0.0041110000
_diffrn_orient_matrix_UB_33      0.0671110000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43475
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.051
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.207
_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    2.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             2800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/pentane'
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0518P)^2^+19.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6833
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_Toluene
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248663
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.243
_diffrn_oxdiff_digest_frames
;
013280eb7686c27c7a1edf228fa3b87075037709371
;
_diffrn_oxdiff_digest_hkl
;
0175935cb213e272576273ff4812688659f960
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116)
2.b Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C117(H11A,H11B,H11C)
;
_shelx_res_checksum              19932
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.657