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_7248653
_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         '2(C22 H16 Ag2 F10 O8), C2 H4 O'
_chemical_formula_sum            'C46 H36 Ag4 F20 O17'
_chemical_formula_weight         1672.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.41420(10)
_cell_length_b                   23.84770(10)
_cell_length_c                   15.13720(10)
_cell_measurement_reflns_used    52036
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5460
_cell_measurement_theta_min      3.4410
_cell_volume                     5194.58(5)
_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_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   -112.00 -20.00   0.50    0.35    --  -87.58  77.00-180.00  184
  2  \w   -122.00 -74.00   0.50    0.12    --  -51.89-125.00   0.00   96
  3  \w   -158.00 -74.00   0.50    0.35    --  -87.58-125.00  60.00  168
  4  \w   -155.00 -86.00   0.50    0.35    --  -87.58 -99.00 150.00  138
  5  \w    -54.00 -13.00   0.50    0.35    --  -87.58  57.00 120.00   82
  6  \w   -129.00 -37.00   0.50    0.12    --  -51.89 -38.00 -30.00  184
  7  \w   -165.00 -73.00   0.50    0.35    --  -90.00 -55.00-136.67  184
  8  \w     28.00  79.00   0.50    0.35    --  102.12 -57.00-180.00  102
  9  \w     52.00  78.00   0.50    0.35    --  102.12 -57.00 -90.00   52
 10  \w     25.00  52.00   0.50    0.35    --  102.12 -38.00   0.00   54
 11  \w     41.00  75.00   0.50    0.35    --  102.12 -57.00  60.00   68
 12  \w     52.00  78.00   0.50    0.35    --  102.12 -57.00  90.00   52
 13  \w     28.00  79.00   0.50    0.35    --  102.12 -57.00 150.00  102
 14  \w     25.00  52.00   0.50    0.35    --  102.12 -38.00 -60.00   54
 15  \w     25.00  52.00   0.50    0.35    --  102.12 -38.00-120.00   54
 16  \w     25.00  52.00   0.50    0.35    --  102.12 -38.00 -90.00   54
 17  \w     71.00 105.00   0.50    0.35    --  102.12 -99.00 -30.00   68
 18  \w     19.00 105.00   0.50    0.12    --   52.14-125.00 -60.00  172
 19  \w     19.00 105.00   0.50    0.12    --   52.14-125.00  30.00  172
 20  \w     32.00 111.00   0.50    0.35    --  102.12-125.00 -60.00  158
 21  \w     32.00 111.00   0.50    0.35    --  102.12-125.00 -90.00  158
 22  \w     32.00 111.00   0.50    0.35    --  102.12-125.00 -30.00  158
 23  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00   0.00  142
 24  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00 120.00  142
 25  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00 150.00  142
 26  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00  90.00  142
 27  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00  30.00  142
 28  \w     35.00 103.00   0.50    0.35    --  102.12 -99.00  60.00  136
 29  \w     35.00  71.00   0.50    0.35    --  102.12 -99.00 -90.00   72
 30  \w     63.00 102.00   0.50    0.35    --  102.12 -99.00-150.00   78
 31  \w     35.00 106.00   0.50    0.35    --  102.12 -99.00-180.00  142
 32  \w     45.00 106.00   0.50    0.35    --  102.12 -99.00-120.00  122
 33  \w     75.00 106.00   0.50    0.35    --  102.12 -99.00 -90.00   62
 34  \w     63.00 176.00   0.50    0.35    --  102.12  19.00 120.00  226
 35  \w     88.00 176.00   0.50    0.35    --  102.12  38.00 150.00  176
 36  \w     34.00 126.00   0.50    0.12    --   58.00  76.00  51.76  184
 37  \w     34.00 125.00   0.50    0.12    --   58.00  77.00 -29.55  182
 38  \w     95.00 159.00   0.50    0.35    --  107.25  71.00 -11.95  128
 39  \w     63.00 176.00   0.50    0.35    --  102.12  19.00  30.00  226
 40  \w     63.00 176.00   0.50    0.35    --  102.12  19.00-120.00  226
;
_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      -0.0519150000
_diffrn_orient_matrix_UB_12      -0.0001315000
_diffrn_orient_matrix_UB_13      0.0861504000
_diffrn_orient_matrix_UB_21      -0.0004688000
_diffrn_orient_matrix_UB_22      -0.0646088000
_diffrn_orient_matrix_UB_23      -0.0005185000
_diffrn_orient_matrix_UB_31      0.0935770000
_diffrn_orient_matrix_UB_32      -0.0004122000
_diffrn_orient_matrix_UB_33      0.0545517000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            104563
_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         74.484
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.251
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    2.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dioxane/pentane'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         10607
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0208P)^2^+5.1388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9585
_reflns_number_total             10607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           Dioxane
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_database_code               7248653
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.220
_diffrn_oxdiff_digest_frames
;
0199c19be5d81067b084219bc2757e253c051840903
;
_diffrn_oxdiff_digest_hkl
;
0164cc0cec65045f6725b98cf43bcbbadd1789
;
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Ag2A \\sim O121 \\sim C122 \\sim C126 \\sim C172 \\sim C176: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O121) = Uanis(O171)
3. Others
 Sof(Ag2A)=Sof(O171)=Sof(C172)=Sof(H17A)=Sof(H17B)=Sof(C176)=Sof(H17C)=
 Sof(H17D)=1-FVAR(1)
 Sof(Ag2)=Sof(O121)=Sof(C122)=Sof(H12A)=Sof(H12B)=Sof(C126)=Sof(H12C)=
 Sof(H12D)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C103(H10C,H10D), C105(H10E,H10F), C106(H10G,H10H), C112(H11A,
 H11B), C116(H11C,H11D), C122(H12A,H12B), C126(H12C,H12D), C132(H13A,H13B),
 C136(H13C,H13D), C142(H14A,H14B), C143(H14C,H14D), C145(H14E,H14F), C146(H14G,
 H14H), C152(H15A,H15B), C156(H15C,H15D), C162(H16A,H16B), C166(H16C,H16D),
 C172(H17A,H17B), C176(H17C,H17D)
;
_shelx_res_checksum              54972
_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 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.849