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_7248662
_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         'C41 H36 Ag3 F15 O8'
_chemical_formula_sum            'C41 H36 Ag3 F15 O8'
_chemical_formula_weight         1265.31
_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             2023-11-10
_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                85.3721(16)
_cell_angle_beta                 70.664(2)
_cell_angle_gamma                86.9586(16)
_cell_formula_units_Z            2
_cell_length_a                   12.4062(3)
_cell_length_b                   13.45738(19)
_cell_length_c                   13.9666(3)
_cell_measurement_reflns_used    39866
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.3220
_cell_measurement_theta_min      3.2890
_cell_volume                     2192.23(8)
_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      120.00(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 0.997
_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    -27.00  26.00   0.50    0.05    --  -51.89  38.00  60.00  106
  2  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00   0.00   82
  3  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00 -30.00   82
  4  \w    -54.00 -13.00   0.50    0.05    --  -87.61  57.00 -90.00   82
  5  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00 -30.00   58
  6  \w     -4.00  25.00   0.50    0.05    --  -51.89  19.00 120.00   58
  7  \w     36.00 127.00   0.50    0.05    --   52.14-158.00 160.00  182
  8  \w     36.00 134.00   0.50    0.05    --  102.08-158.00 160.00  196
  9  \w     36.00  78.00   0.50    0.05    --  102.08-125.00  90.00   84
 10  \w     32.00  79.00   0.50    0.05    --  102.08-125.00 120.00   94
 11  \w     33.00 109.00   0.50    0.05    --  102.08-119.00 -45.00  152
 12  \w     35.00 106.00   0.50    0.05    --  102.08 -99.00   0.00  142
 13  \w     32.00 107.00   0.50    0.05    --  102.08-125.00 -60.00  150
 14  \w     32.00 111.00   0.50    0.05    --  102.08-125.00 -90.00  158
 15  \w     47.00  89.00   0.50    0.05    --  102.08-125.00-120.00   84
 16  \w     52.00 103.00   0.50    0.05    --  102.08 -99.00-180.00  102
 17  \w     55.00 104.00   0.50    0.05    --  102.08 -99.00 -60.00   98
 18  \w     15.00 100.00   0.50    0.05    --   52.14-119.00 -45.00  170
 19  \w     74.00 100.00   0.50    0.05    --  102.08 -99.00  30.00   52
 20  \w     65.00 106.00   0.50    0.05    --  102.08 -99.00  60.00   82
 21  \w     37.00 101.00   0.50    0.05    --  102.08 -99.00 120.00  128
 22  \w     50.00 106.00   0.50    0.05    --  102.08 -99.00 150.00  112
 23  \w     74.00 105.00   0.50    0.05    --  102.08 -99.00 -30.00   62
 24  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00   0.00  102
 25  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00 -60.00   54
 26  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00 -90.00  102
 27  \w     43.00  78.00   0.50    0.05    --  102.08 -57.00-150.00   70
 28  \w     25.00  52.00   0.50    0.05    --  102.08 -38.00-180.00   54
 29  \w     25.00  50.00   0.50    0.05    --  102.08 -38.00 -30.00   50
 30  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00 -30.00  102
 31  \w     28.00  79.00   0.50    0.05    --  102.08 -57.00 150.00  102
 32  \w     25.00  51.00   0.50    0.05    --  102.08 -38.00  90.00   52
 33  \w     64.00 100.00   0.50    0.05    --  102.08  19.00   0.00   72
 34  \w     94.00 120.00   0.50    0.05    --  102.08  38.00 -30.00   52
 35  \w    130.00 157.00   0.50    0.05    --  102.08  38.00 -30.00   54
 36  \w     88.00 171.00   0.50    0.05    --  102.08  38.00-180.00  166
 37  \w     46.00 137.00   0.50    0.05    --   70.00  77.00   2.60  182
 38  \w    132.00 158.00   0.50    0.05    --  102.08  19.00   0.00   52
 39  \w     63.00 176.00   0.50    0.05    --  102.08  19.00 120.00  226
 40  \w     84.00 172.00   0.50    0.05    --  102.08 119.00  39.00  176
 41  \w     58.00 160.00   0.50    0.05    --  102.08 158.00-165.00  204
 42  \w     82.00 123.00   0.50    0.05    --  102.08 125.00-180.00   82
 43  \w    136.00 162.00   0.50    0.05    --  102.08 125.00-180.00   52
 44  \w     58.00 119.00   0.50    0.05    --   52.14 158.00-165.00  122
 45  \w   -127.00 -30.00   0.50    0.05    --  -51.89 158.00-165.00  194
 46  \w   -109.00 -18.00   0.50    0.05    --  -87.61 119.00  39.00  182
 47  \w   -100.00  -9.00   0.50    0.05    --  -51.89 119.00  39.00  182
 48  \w   -134.00 -30.00   0.50    0.05    --  -87.61 158.00-165.00  208
 49  \w   -119.00 -27.00   0.50    0.05    --  -51.89 -77.00-180.00  184
 50  \w   -157.00 -78.00   0.50    0.05    --  -87.61-119.00 -45.00  158
 51  \w   -158.00 -74.00   0.50    0.05    --  -87.61-125.00   0.00  168
 52  \w   -118.00 -51.00   0.50    0.05    --  -51.89-158.00 160.00  134
 53  \w   -154.00 -51.00   0.50    0.05    --  -87.61-158.00 160.00  206
;
_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      0.0017696000
_diffrn_orient_matrix_UB_12      0.1138334000
_diffrn_orient_matrix_UB_13      -0.0236346000
_diffrn_orient_matrix_UB_21      0.1315676000
_diffrn_orient_matrix_UB_22      -0.0052349000
_diffrn_orient_matrix_UB_23      -0.0416964000
_diffrn_orient_matrix_UB_31      -0.0043326000
_diffrn_orient_matrix_UB_32      -0.0146895000
_diffrn_orient_matrix_UB_33      -0.1069078000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.484
_diffrn_reflns_theta_min         3.296
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.697
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.197
_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    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: eucalyptol/pentane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.537
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         8953
_refine_ls_number_restraints     705
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0413P)^2^+4.4489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8507
_reflns_number_total             8953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00441h2.cif
_cod_data_source_block           1_Eucalyptol
_cod_depositor_comments
'Adding full bibliography for 7248652--7248666.cif.'
_cod_original_cell_volume        2192.24(8)
_cod_database_code               7248662
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.227
_diffrn_oxdiff_digest_frames
;
014ed71eaef849cada2d1add62f1e8972906260d1c0
;
_diffrn_oxdiff_digest_hkl
;
01c28c81c0349c479c005333a233c31e6577cd
;
_reflns_odcompleteness_completeness 99.74
_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, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 F100, F101, F102, F103, F104, C94, C95, C96, C97, C98, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F40, F41, F42, F43, F44, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O201, C203, C209, C212, C214, C215, C216, C217, C218, C220, C221
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O201, C202, C203, C204, C205, C206, C207, C208, C209, C210, C211
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F120, F121, F122, F123, F124, C114, C115, C116, C117, C118, C119
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F20, F21, F22, F23, F24, C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F60, F61, F62, F63, F64, C52, C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
3. Others
 Sof(C202)=Sof(H20A)=Sof(C204)=Sof(H20B)=Sof(H20C)=Sof(C205)=Sof(H20D)=
 Sof(H20E)=Sof(C206)=Sof(C207)=Sof(H20F)=Sof(H20G)=Sof(C208)=Sof(H20H)=
 Sof(H20I)=Sof(H20M)=Sof(H20N)=Sof(H20O)=Sof(C210)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C211)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H203)=Sof(H20J)=Sof(H20K)=Sof(H20L)=Sof(C212)=Sof(C214)=Sof(H21G)=
 Sof(H21H)=Sof(C215)=Sof(H21I)=Sof(H21J)=Sof(C216)=Sof(C217)=Sof(H21K)=
 Sof(H21L)=Sof(C218)=Sof(H21M)=Sof(H21N)=Sof(C220)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C221)=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(1)
 Sof(F40)=Sof(F41)=Sof(F42)=Sof(F43)=Sof(F44)=Sof(C36)=Sof(C35)=Sof(C34)=
 Sof(C39)=Sof(C38)=Sof(C37)=1-FVAR(2)
 Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(C14)=Sof(C15)=Sof(C16)=
 Sof(C17)=Sof(C18)=Sof(C19)=FVAR(2)
 Sof(F80)=Sof(F81)=Sof(F82)=Sof(F83)=Sof(F84)=Sof(C79)=Sof(C74)=Sof(C75)=
 Sof(C76)=Sof(C77)=Sof(C78)=1-FVAR(3)
 Sof(F60)=Sof(F61)=Sof(F62)=Sof(F63)=Sof(F64)=Sof(C59)=Sof(C54)=Sof(C55)=
 Sof(C56)=Sof(C57)=Sof(C58)=FVAR(3)
 Sof(F120)=Sof(F121)=Sof(F122)=Sof(F123)=Sof(F124)=Sof(C119)=Sof(C118)=
 Sof(C117)=Sof(C116)=Sof(C115)=Sof(C114)=1-FVAR(4)
 Sof(F100)=Sof(F101)=Sof(F102)=Sof(F103)=Sof(F104)=Sof(C99)=Sof(C98)=Sof(C97)=
 Sof(C96)=Sof(C95)=Sof(C94)=FVAR(4)
4.a Ternary CH refined with riding coordinates:
 C203(H203), C203(H20A), C233(H233)
4.b Secondary CH2 refined with riding coordinates:
 C204(H20B,H20C), C205(H20D,H20E), C207(H20F,H20G), C208(H20H,H20I), C214(H21G,
 H21H), C215(H21I,H21J), C217(H21K,H21L), C218(H21M,H21N), C234(H23A,H23B),
 C235(H23C,H23D), C237(H23E,H23F), C238(H23G,H23H)
4.c Fitted hexagon refined as free rotating group:
 C36(C35,C34,C39,C38,C37), C59(C54,C55,C56,C57,C58), C79(C74,C75,C76,C77,C78),
 C99(C98,C97,C96,C95,C94), C119(C118,C117,C116,C115,C114)
4.d Idealised Me refined as rotating group:
 C209(H20J,H20K,H20L), C209(H20M,H20N,H20O), C210(H21A,H21B,H21C), C211(H21D,
 H21E,H21F), C220(H22A,H22B,H22C), C221(H22D,H22E,H22F), C239(H23I,H23J,H23K),
 C240(H24A,H24B,H24C), C241(H24D,H24E,H24F)
;
_shelx_res_checksum              86684
_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 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.873