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_7248664
_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         'C12 H10 Ag F5 O3'
_chemical_formula_sum            'C12 H10 Ag F5 O3'
_chemical_formula_weight         405.07
_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             2023-10-27
_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                75.275(3)
_cell_angle_beta                 85.880(2)
_cell_angle_gamma                79.845(3)
_cell_formula_units_Z            2
_cell_length_a                   5.51822(13)
_cell_length_b                   9.8945(5)
_cell_length_c                   13.0489(3)
_cell_measurement_reflns_used    10046
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.7070
_cell_measurement_theta_min      3.4910
_cell_volume                     678.00(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_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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   -116.00 -21.00   0.50    0.10    --  -41.67 140.00 118.00  190
  2  \w   -121.00 -72.00   0.50    0.10    --  -41.67-130.00-126.00   98
  3  \w   -110.00 -16.00   0.50    0.10    --  -41.67 130.00 -55.00  188
  4  \w   -120.00 -65.00   0.50    0.10    --  -41.67-140.00  59.00  110
  5  \w     22.00 111.00   0.50    0.10    --   42.36-130.00-126.00  178
  6  \w     71.00 121.00   0.50    0.10    --   42.36 140.00 118.00  100
  7  \w     28.00 117.00   0.50    0.10    --   42.36-140.00  59.00  178
  8  \w   -122.00 -21.00   0.50    0.60    --  -89.36 140.00 118.00  202
  9  \w   -115.00 -16.00   0.50    0.60    --  -89.36 130.00 -55.00  198
 10  \w   -170.00 -71.00   0.50    0.60    --  -89.36-130.00-126.00  198
 11  \w     70.00 173.00   0.50    0.60    --  113.01 140.00 118.00  206
 12  \w     32.00 116.00   0.50    0.60    --  113.01-130.00-126.00  168
 13  \w     77.00 176.00   0.50    0.60    --  113.01 130.00 -55.00  198
 14  \w     34.00 123.00   0.50    0.60    --  113.01-140.00  59.00  178
 15  \w     -4.00  45.00   0.50    0.10    --  -41.67  19.00 -30.00   98
 16  \w    -27.00  45.00   0.50    0.10    --  -41.67  38.00 -30.00  144
 17  \w     12.00 124.00   0.50    0.10    --   42.36  57.00-180.00  224
 18  \w      2.00  28.00   0.50    0.10    --   50.00  96.00 -36.57   52
 19  \w      7.00  34.00   0.50    0.10    --   54.00  94.00 125.28   54
 20  \w   -153.00 -42.00   0.50    0.10    --  -78.00 -74.00-109.69  222
 21  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00 -30.00   64
 22  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00-180.00   64
 23  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00-150.00   64
 24  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00 -60.00   64
 25  \w   -127.00 -16.00   0.50    0.60    --  -89.36  77.00 150.00  222
 26  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00 120.00   64
 27  \w    -37.00  -5.00   0.50    0.60    --  -89.36  45.00  90.00   64
 28  \w   -174.00 -69.00   0.50    0.60    --  -95.50 -45.00  98.07  210
 29  \w     33.00 111.00   0.50    0.60    --  113.01-125.00 150.00  156
 30  \w     33.00 111.00   0.50    0.60    --  113.01-125.00 -90.00  156
 31  \w     33.00  86.00   0.50    0.60    --  113.01 -61.00-120.00  106
 32  \w     67.00 176.00   0.50    0.60    --  113.01  30.00   0.00  218
 33  \w     33.00  86.00   0.50    0.60    --  113.01 -61.00   0.00  106
 34  \w     28.00  62.00   0.50    0.60    --  113.01 -45.00   0.00   68
 35  \w     80.00 176.00   0.50    0.60    --  113.01 125.00  30.00  192
 36  \w     80.00 176.00   0.50    0.60    --  113.01 125.00-180.00  192
 37  \w     33.00  86.00   0.50    0.60    --  113.01 -61.00 -90.00  106
 38  \w     87.00 176.00   0.50    0.60    --  113.01  45.00 -60.00  178
 39  \w     33.00 111.00   0.50    0.60    --  113.01-125.00 -30.00  156
 40  \w     28.00  62.00   0.50    0.60    --  113.01 -45.00-180.00   68
 41  \w     32.00 105.00   0.50    0.60    --  113.01 -95.00 150.00  146
 42  \w     28.00  62.00   0.50    0.60    --  113.01 -45.00 120.00   68
 43  \w     33.00  86.00   0.50    0.60    --  113.01 -61.00 120.00  106
 44  \w     28.00  62.00   0.50    0.60    --  113.01 -45.00 -90.00   68
 45  \w     28.00  62.00   0.50    0.60    --  113.01 -45.00-150.00   68
 46  \w     87.00 176.00   0.50    0.60    --  113.01  45.00  30.00  178
 47  \w     32.00 105.00   0.50    0.60    --  113.01 -95.00   0.00  146
 48  \w     33.00  86.00   0.50    0.60    --  113.01 -61.00  60.00  106
 49  \w     12.00 124.00   0.50    0.10    --   42.36  57.00   0.00  224
 50  \w     14.00 125.00   0.50    0.10    --   50.00  75.00 -92.95  222
 51  \w      5.00  41.00   0.50    0.10    --   50.00  91.00  80.92   72
 52  \w      9.00  41.00   0.50    0.10    --   54.00  91.00 179.38   64
 53  \w      7.00  34.00   0.50    0.10    --   54.00  94.00-133.81   54
 54  \w     14.00  42.00   0.50    0.10    --   58.00  88.00  -8.06   56
 55  \w     13.00  41.00   0.50    0.10    --   58.00  91.00  33.57   56
 56  \w   -145.00 -34.00   0.50    0.10    --  -66.00 -65.00  72.85  222
 57  \w   -163.00 -52.00   0.50    0.60    --  -89.36 -77.00   0.00  222
 58  \w   -163.00 -52.00   0.50    0.60    --  -89.36 -77.00  60.00  222
 59  \w   -171.00 -61.00   0.50    0.60    --  -95.50 -72.00 176.28  220
 60  \w     76.00 176.00   0.50    0.60    --  113.01  77.00  90.00  200
 61  \w     67.00 176.00   0.50    0.60    --  113.01  30.00 -90.00  218
;
_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      0.2829411000
_diffrn_orient_matrix_UB_12      -0.0375901000
_diffrn_orient_matrix_UB_13      0.0023390000
_diffrn_orient_matrix_UB_21      -0.0128771000
_diffrn_orient_matrix_UB_22      -0.0338407000
_diffrn_orient_matrix_UB_23      0.1220171000
_diffrn_orient_matrix_UB_31      -0.0168469000
_diffrn_orient_matrix_UB_32      -0.1551557000
_diffrn_orient_matrix_UB_33      0.0044174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16388
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.504
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.592
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.270
_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    1.984
_exptl_crystal_description       needle
_exptl_crystal_F_000             396
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 2-methyltetrahydrofuran (racemic)/pentane'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0687P)^2^+0.3722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2470
_reflns_number_total             2742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_2-MeTHF
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248664
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.235
_diffrn_oxdiff_digest_frames
;
016cb5cba3d5a12b367a4ffdb9688d9c7a08640a26e
;
_diffrn_oxdiff_digest_hkl
;
014a30f6f1b72cbf6410635d038f75c62a69bf
;
_reflns_odcompleteness_completeness 99.38
_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. Restrained distances
 C113-C114 = C104-C103 = C115-C114
 1.52 with sigma of 0.02
 C104-C105 = C112-C113
 1.52 with sigma of 0.01
 C102-C103
 1.52 with sigma of 0.01
 C112-C116 = C102-C106
 1.52 with sigma of 0.02
 O101-C105 = O111-C115 = O111-C112 = O101-C102
 1.44 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O101 \\sim O111 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C112 \\sim
C113 \\sim C114 \\sim C115 \\sim C116: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C103) = Uanis(C102)
4. Others
 Sof(O111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H11A)=Sof(H11B)=Sof(C114)=
 Sof(H11C)=Sof(H11D)=Sof(C115)=Sof(H11E)=Sof(H11F)=Sof(C116)=Sof(H11G)=
 Sof(H11H)=Sof(H11I)=1-FVAR(1)
 Sof(O101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H10A)=Sof(H10B)=Sof(C104)=
 Sof(H10C)=Sof(H10D)=Sof(C105)=Sof(H10E)=Sof(H10F)=Sof(C106)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C102(H102), C112(H112)
5.b Secondary CH2 refined with riding coordinates:
 C103(H10A,H10B), C104(H10C,H10D), C105(H10E,H10F), C113(H11A,H11B), C114(H11C,
 H11D), C115(H11E,H11F)
5.c Idealised Me refined as rotating group:
 C106(H10G,H10H,H10I), C116(H11G,H11H,H11I)
;
_shelx_res_checksum              81970
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.637