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_7248660
_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         'C32 H20 Ag2 F10 O6, 2(C9 H10 O)'
_chemical_formula_sum            'C50 H40 Ag2 F10 O8'
_chemical_formula_weight         1174.56
_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             2024-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                85.841(4)
_cell_angle_beta                 85.713(3)
_cell_angle_gamma                84.263(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2534(3)
_cell_length_b                   11.0121(5)
_cell_length_c                   13.8225(6)
_cell_measurement_reflns_used    12381
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      76.2500
_cell_measurement_theta_min      3.1970
_cell_volume                     1093.11(8)
_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(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_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    -54.00 -13.00   0.50    0.10    --  -87.66  57.00  60.00   82
  2  \w   -112.00 -36.00   0.50    0.10    --  -87.66  77.00-150.00  152
  3  \w   -112.00 -36.00   0.50    0.10    --  -87.66  77.00-150.00  152
  4  \w    -58.00 -14.00   0.50    0.10    --  -87.66  59.00-166.00   88
  5  \w    -58.00  22.00   0.50    0.05    --  -51.43  59.00-166.00  160
  6  \w     -4.00  25.00   0.50    0.05    --  -51.43  19.00 -90.00   58
  7  \w    -54.00 -13.00   0.50    0.10    --  -87.66  57.00 120.00   82
  8  \w     -4.00  25.00   0.50    0.05    --  -51.43  19.00 120.00   58
  9  \w     63.00 106.00   0.50    0.10    --  102.08  19.00-180.00   86
 10  \w     85.00 176.00   0.50    0.10    --  102.08  59.00-166.00  182
 11  \w     83.00 161.00   0.50    0.10    --  102.08  77.00-150.00  156
 12  \w     34.00 126.00   0.50    0.05    --   51.81  59.00-166.00  184
 13  \w     34.00 126.00   0.50    0.05    --   51.81  59.00-166.00  184
 14  \w    129.00 165.00   0.50    0.10    --  102.08  19.00-180.00   72
 15  \w     85.00 176.00   0.50    0.10    --  102.08  59.00-166.00  182
 16  \w    126.00 152.00   0.50    0.10    --  102.08  57.00 -60.00   52
 17  \w    122.00 168.00   0.50    0.10    --  102.08  77.00 120.00   92
 18  \w     78.00 113.00   0.50    0.10    --  102.08  77.00 120.00   70
 19  \w    119.00 168.00   0.50    0.10    --  102.08 125.00 120.00   98
 20  \w     81.00 149.00   0.50    0.10    --  102.08 125.00  60.00  136
 21  \w     81.00 152.00   0.50    0.10    --  102.08 125.00  30.00  142
 22  \w    -54.00 -28.00   0.50    0.05    --   18.00 154.00-129.49   52
 23  \w     26.00  52.00   0.50    0.10    --  102.08 -38.00   0.00   52
 24  \w     29.00  73.00   0.50    0.10    --  102.08 -57.00   0.00   88
 25  \w    101.00 127.00   0.50    0.10    --  102.08 -77.00  60.00   52
 26  \w     47.00  73.00   0.50    0.10    --  102.08 -57.00 -60.00   52
 27  \w    -22.00  70.00   0.50    0.05    --   51.81 -59.00  53.00  184
 28  \w     29.00  83.00   0.50    0.10    --  102.08 -59.00  53.00  108
 29  \w     35.00  70.00   0.50    0.10    --  102.08 -77.00  60.00   70
 30  \w     68.00 110.00   0.50    0.10    --  102.08-125.00  60.00   84
 31  \w     65.00  98.00   0.50    0.10    --  102.08 -99.00  60.00   66
 32  \w     34.00  59.00   0.50    0.10    --  102.08-125.00  60.00   50
 33  \w     35.00 102.00   0.50    0.10    --  102.08 -99.00 -30.00  134
 34  \w     34.00  90.00   0.50    0.10    --  102.08-125.00 -30.00  112
 35  \w     38.00  67.00   0.50    0.10    --  102.08 -99.00 -90.00   58
 36  \w     71.00 106.00   0.50    0.10    --  102.08 -99.00 -90.00   70
 37  \w     74.00 106.00   0.50    0.10    --  102.08 -99.00-150.00   64
 38  \w     68.00  94.00   0.50    0.10    --  102.08 -99.00-120.00   52
 39  \w     44.00  69.00   0.50    0.10    --  102.08 -99.00-150.00   50
 40  \w     36.00  66.00   0.50    0.10    --  102.08 -99.00-120.00   60
 41  \w     35.00  96.00   0.50    0.10    --  102.08 -99.00-180.00  122
 42  \w     75.00 106.00   0.50    0.10    --  102.08 -99.00  90.00   62
 43  \w     44.00  70.00   0.50    0.10    --  102.08 -99.00 120.00   52
 44  \w     80.00 106.00   0.50    0.10    --  102.08 -99.00 120.00   52
 45  \w   -112.00 -17.00   0.50    0.10    --  -87.66 125.00-150.00  190
 46  \w   -112.00 -17.00   0.50    0.10    --  -87.66 125.00 -60.00  190
 47  \w   -112.00 -17.00   0.50    0.10    --  -87.66 125.00 -60.00  190
 48  \w   -155.00 -86.00   0.50    0.10    --  -87.66 -99.00-180.00  138
 49  \w   -122.00 -74.00   0.50    0.05    --  -51.43-125.00-150.00   96
 50  \w   -161.00 -70.00   0.50    0.10    --  -87.66 -59.00  53.00  182
 51  \w   -125.00 -34.00   0.50    0.05    --  -51.43 -59.00  53.00  182
;
_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      -0.1867775000
_diffrn_orient_matrix_UB_12      -0.0427697000
_diffrn_orient_matrix_UB_13      0.0427042000
_diffrn_orient_matrix_UB_21      0.0262880000
_diffrn_orient_matrix_UB_22      -0.1083619000
_diffrn_orient_matrix_UB_23      -0.0657921000
_diffrn_orient_matrix_UB_31      0.1009997000
_diffrn_orient_matrix_UB_32      -0.0792632000
_diffrn_orient_matrix_UB_33      0.0799585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22573
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.213
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.081
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (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    1.784
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: isochroman/pentane'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0223P)^2^+1.8871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3829
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_Isochroman
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248660
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.470
_diffrn_oxdiff_digest_frames
;
0156087976f892603c4c41124f633d95ce05382900b
;
_diffrn_oxdiff_digest_hkl
;
01259247f51222d955eb688519bb5886a4e904
;
_reflns_odcompleteness_completeness 99.51
_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
2. Restrained distances
 C59A-C53 = C59A-C60A
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O51A, C53, C58, C59, C59A, C60A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O51A)=Sof(H59C)=Sof(H59D)=Sof(C59A)=Sof(H59E)=Sof(H59F)=Sof(C60A)=
 Sof(H60C)=Sof(H60D)=1-FVAR(1)
 Sof(O51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=FVAR(1)
 Sof(O31A)=Sof(H32C)=Sof(H32D)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=1-FVAR(2)
 Sof(O31)=Sof(H32A)=Sof(H32B)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32C,H32D), C32(H32A,H32B), C39(H39A,H39B), C39(H39C,H39D), C40(H40A,
 H40B), C40A(H40C,H40D), C52(H52A,H52B), C59(H59A,H59B), C59(H59C,H59D),
 C59A(H59E,H59F), C60(H60A,H60B), C60A(H60C,H60D)
5.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C37(H37), C54(H54), C55(H55), C56(H56), C57(H57)
;
_shelx_res_checksum              51604
_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 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.605