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_7248659
_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_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_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