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_7248655
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H14 Ag2 F10 O5'
_chemical_formula_sum            'C24 H14 Ag2 F10 O5'
_chemical_formula_weight         788.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-29 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5758(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.79831(19)
_cell_length_b                   5.58069(5)
_cell_length_c                   25.9618(2)
_cell_measurement_reflns_used    19440
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1290
_cell_measurement_theta_min      3.4970
_cell_volume                     2495.71(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)'
_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 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    -31.00  -5.00   0.50    0.05    --   14.00 114.00 -17.74   52
  2  \w      4.00  34.00   0.50    0.05    --   38.00  94.00  -2.62   60
  3  \w     15.00  42.00   0.50    0.05    --   46.00  89.00 175.16   54
  4  \w      8.00  42.00   0.50    0.05    --   38.00  87.00  97.03   68
  5  \w     28.00 119.00   0.50    0.05    --   52.14  77.00  30.00  182
  6  \w     39.00 130.00   0.50    0.05    --   62.00  75.00  93.47  182
  7  \w     78.00 169.00   0.50    0.05    --  102.08  77.00   0.00  182
  8  \w     28.00 119.00   0.50    0.05    --   52.14  77.00 -90.00  182
  9  \w     42.00 133.00   0.50    0.05    --   66.00  77.00-169.20  182
 10  \w     88.00 176.00   0.50    0.05    --  102.08  38.00 -30.00  176
 11  \w     46.00 138.00   0.50    0.05    --   70.00  76.00 -51.42  184
 12  \w     85.00 176.00   0.50    0.05    --  102.08  57.00  60.00  182
 13  \w     88.00 176.00   0.50    0.05    --  102.08  38.00 120.00  176
 14  \w     81.00 173.00   0.50    0.05    --  102.08 124.00  37.00  184
 15  \w     80.00 173.00   0.50    0.05    --  102.08 125.00   0.00  186
 16  \w     64.00 166.00   0.50    0.05    --  102.08 148.00-158.00  204
 17  \w     80.00 173.00   0.50    0.05    --  102.08 125.00 150.00  186
 18  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00  90.00   54
 19  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00  90.00  102
 20  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00  30.00   54
 21  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00-180.00  102
 22  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00 -90.00   54
 23  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00 -30.00  102
 24  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00  30.00  102
 25  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00 120.00   54
 26  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00  60.00  142
 27  \w     19.00 104.00   0.50    0.05    --   52.14-124.00 -41.00  170
 28  \w     32.00 111.00   0.50    0.05    --  102.08-125.00 -60.00  158
 29  \w     32.00 111.00   0.50    0.05    --  102.08-125.00 -30.00  158
 30  \w     32.00 111.00   0.50    0.05    --  102.08-124.00 -41.00  158
 31  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00-150.00  142
 32  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00 -30.00  142
 33  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00-180.00  142
 34  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00   0.00  142
 35  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00 -60.00  142
 36  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00 120.00  142
 37  \w     32.00 120.00   0.50    0.05    --   52.14-148.00 154.00  176
 38  \w     33.00 128.00   0.50    0.05    --  102.08-148.00 154.00  190
 39  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00   0.00   58
 40  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00  90.00   58
 41  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00  30.00   82
 42  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00   0.00   82
 43  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00  60.00   58
 44  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00 150.00   58
 45  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00-120.00   82
 46  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00-180.00   58
 47  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00-150.00   82
 48  \w   -128.00 -25.00   0.50    0.05    --  -87.61 148.00-158.00  206
 49  \w   -164.00 -73.00   0.50    0.05    --  -95.50 -74.00-104.61  182
 50  \w   -137.00 -45.00   0.50    0.05    --  -70.00 -77.00  -2.83  184
 51  \w   -151.00 -60.00   0.50    0.05    --  -82.00 -72.00 165.94  182
 52  \w   -166.00-119.00   0.50    0.05    --  -95.50 -69.00 151.26   94
 53  \w   -121.00 -58.00   0.50    0.05    --  -51.89-148.00 154.00  126
 54  \w   -157.00 -58.00   0.50    0.05    --  -87.61-148.00 154.00  198
 55  \w   -122.00 -75.00   0.50    0.05    --  -51.89-124.00 -41.00   94
 56  \w   -158.00 -75.00   0.50    0.05    --  -87.61-124.00 -41.00  166
;
_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      0.0081914000
_diffrn_orient_matrix_UB_12      0.2749093000
_diffrn_orient_matrix_UB_13      0.0015492000
_diffrn_orient_matrix_UB_21      0.0315668000
_diffrn_orient_matrix_UB_22      -0.0095861000
_diffrn_orient_matrix_UB_23      0.0609372000
_diffrn_orient_matrix_UB_31      0.0832776000
_diffrn_orient_matrix_UB_32      -0.0234577000
_diffrn_orient_matrix_UB_33      -0.0066392000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35933
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.482
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    2.097
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: R-carvone/pentane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2002 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         5084
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4748
_reflns_number_total             5084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_R_Carvone
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248655
_shelxl_version_number           2014/6
_diffrn_oxdiff_digest_frames
;
012047cce390550a4ebb3924f6e4a141ba073002b06
;
_diffrn_oxdiff_digest_hkl
;
01c790cd13631318627279fffe9faa2a1819fa
;
_reflns_odcompleteness_completeness 99.75
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C126 \\sim C129 \\sim C130 \\sim C131 \\sim C140 \\sim C141: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(Ag3)=Sof(Ag4)=Sof(O121)=Sof(C122)=Sof(C123)=Sof(C124)=Sof(H124)=Sof(C125)=
 Sof(H12A)=Sof(H12B)=Sof(C126)=Sof(H126)=Sof(C127)=Sof(H12C)=Sof(H12D)=
 Sof(C128)=Sof(H12E)=Sof(H12F)=Sof(H12G)=Sof(C129)=1-FVAR(1)
 Sof(Ag1)=Sof(Ag2)=Sof(O101)=Sof(C102)=Sof(C103)=Sof(C104)=Sof(H104)=Sof(C105)=
 Sof(H10A)=Sof(H10B)=Sof(C106)=Sof(H106)=Sof(C107)=Sof(H10C)=Sof(H10D)=
 Sof(C108)=Sof(H10E)=Sof(H10F)=Sof(H10G)=Sof(C109)=Sof(C110)=Sof(H11A)=
 Sof(H11B)=Sof(C111)=Sof(H11C)=Sof(H11D)=Sof(H11E)=FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(H14D)=Sof(H14E)=Sof(C140)=Sof(C141)=0.51051*
 (1-FVAR(3))
 Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(C131)=Sof(H13C)=Sof(H13D)=Sof(H13E)=0.51051*
 FVAR(3)
 Fixed X: H14A(0.37569) H14B(0.42795) H14C(0.437599) H14D(0.367841)
 H14E(0.35248)
 Fixed Y: H14A(0.95237) H14B(0.896549) H14C(0.40167) H14D(0.4928) H14E(0.29155)
 Fixed Z: H14A(0.288529) H14B(0.34881) H14C(0.36406) H14D(0.3877) H14E(0.34234)
4.a Ternary CH refined with riding coordinates:
 C126(H126), C106(H106)
4.b Secondary CH2 refined with riding coordinates:
 C125(H12A,H12B), C127(H12C,H12D), C105(H10A,H10B), C107(H10C,H10D)
4.c Aromatic/amide H refined with riding coordinates:
 C124(H124), C104(H104)
4.d X=CH2 refined with riding coordinates:
 C130(H13A,H13B), C110(H11A,H11B)
4.e Idealised Me refined as rotating group:
 C128(H12E,H12F,H12G), C131(H13C,H13D,H13E), C108(H10E,H10F,H10G), C111(H11C,
 H11D,H11E)
;
_shelx_res_checksum              2881
_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 2.495
_oxdiff_exptl_absorpt_empirical_full_min 0.742