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_7248665
_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         'C14 H5 Ag2 F5 O4'
_chemical_formula_sum            'C14 H5 Ag2 F5 O4'
_chemical_formula_weight         547.92
_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             2023-10-25
_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                 93.837(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9141(3)
_cell_length_b                   5.5610(2)
_cell_length_c                   37.1068(11)
_cell_measurement_reflns_used    5182
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.7990
_cell_measurement_theta_min      2.3800
_cell_volume                     1423.53(9)
_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_temperature      120.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   -107.00 -15.00   0.50    0.80    --  -51.51 129.00  38.00  184
  2  \w   -122.00 -62.00   0.50    0.80    --  -51.51-142.00 153.00  120
  3  \w   -123.00 -71.00   0.50    0.80    --  -51.51-129.00 -34.00  104
  4  \w     22.00 107.00   0.50    0.80    --   51.89-129.00 -34.00  170
  5  \w   -159.00 -71.00   0.50    3.20    --  -87.61-129.00 -34.00  176
  6  \w   -115.00 -19.00   0.50    3.20    --  -87.61 129.00  38.00  192
  7  \w   -110.00 -76.00   0.50    3.20    --  -87.61-142.00 153.00   68
  8  \w   -123.00 -67.00   0.50    3.20    --  -87.61 142.00-149.00  112
  9  \w     54.00  79.00   0.50    3.20    --  102.08-142.00 153.00   50
 10  \w    103.00 161.00   0.50    3.20    --  102.08 142.00-149.00  116
 11  \w     45.00  78.00   0.50    3.20    --  102.08-129.00 -34.00   66
 12  \w     -3.00  22.00   0.50    0.80    --  -51.51  19.00 -30.00   50
 13  \w     -2.00  23.00   0.50    0.80    --  -51.51  19.00-120.00   50
 14  \w   -141.00 -52.00   0.50    0.80    --  -70.00 -68.00 -20.31  178
 15  \w    -54.00 -20.00   0.50    3.20    --  -87.61  57.00-180.00   68
 16  \w    -54.00 -29.00   0.50    3.20    --  -87.61  57.00  30.00   50
 17  \w   -156.00-127.00   0.50    3.20    --  -95.50 -90.00  70.97   58
 18  \w     88.00 169.00   0.50    3.20    --  102.08  38.00 -90.00  162
 19  \w     37.00 102.00   0.50    3.20    --  102.08 -99.00 -30.00  130
 20  \w     25.00  52.00   0.50    3.20    --  102.08 -38.00-180.00   54
 21  \w    133.00 175.00   0.50    3.20    --  102.08  38.00  30.00   84
 22  \w     80.00 106.00   0.50    3.20    --  102.08 -99.00  60.00   52
 23  \w     90.00 125.00   0.50    3.20    --  102.08  38.00  30.00   70
 24  \w     76.00 104.00   0.50    3.20    --  102.08 -99.00 150.00   56
 25  \w     41.00  77.00   0.50    3.20    --  102.08 -77.00 -30.00   72
 26  \w     89.00 127.00   0.50    3.20    --  102.08 -77.00 -30.00   76
 27  \w     38.00  65.00   0.50    3.20    --  102.08 -99.00 150.00   54
 28  \w     42.00 106.00   0.50    3.20    --  102.08 -99.00 -90.00  128
 29  \w     56.00 104.00   0.50    3.20    --  102.08 -99.00  30.00   96
 30  \w     25.00  50.00   0.50    3.20    --  102.08 -38.00  90.00   50
 31  \w     25.00  52.00   0.50    3.20    --  102.08 -38.00 120.00   54
;
_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      0.0002271000
_diffrn_orient_matrix_UB_12      -0.2764383000
_diffrn_orient_matrix_UB_13      -0.0024460000
_diffrn_orient_matrix_UB_21      -0.1756599000
_diffrn_orient_matrix_UB_22      -0.0101727000
_diffrn_orient_matrix_UB_23      0.0233867000
_diffrn_orient_matrix_UB_31      -0.1379276000
_diffrn_orient_matrix_UB_32      0.0127695000
_diffrn_orient_matrix_UB_33      -0.0343458000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            14758
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.864
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (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    2.557
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dibenzyl ether/pentane'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.013
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0604P)^2^+5.7349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2336
_reflns_number_total             2894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_AgBenzoate
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248665
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.114
_diffrn_oxdiff_digest_frames
;
017e572b6600bb1bf48c2dab0faa973b24029508db6
;
_diffrn_oxdiff_digest_hkl
;
014f5c7372f520ff27ae6e85869923af08707f
;
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_shelx_res_checksum              93814
_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 1.490
_oxdiff_exptl_absorpt_empirical_full_min 0.620