Solvent-free anhydrous Li+, Na+ and K+ salts of [B(3,5-(CF3)2C6H3)4]−, [BArF4]−. Improved synthesis and solid-state structures
Martínez-Martínez, Antonio J.; Weller, Andrew S.; Dalton Transactions  (2019) –; doi:10.1039/C9DT00235A

data_7049019
_publ_section_title
;
 Solvent-free anhydrous Li+, Na+ and K+ salts of
 [B(3,5-(CF3)2C6H3)4]&#x2212;, [BArF4]&#x2212;. Improved synthesis and
 solid-state structures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00235A
_journal_year                    2019
_chemical_formula_moiety         '0.5(C64 H24 B2 F48 Na2)'
_chemical_formula_sum            'C32 H12 B F24 Na'
_chemical_formula_weight         886.22
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3508(2)
_cell_length_b                   13.3508(2)
_cell_length_c                   9.3819(2)
_cell_measurement_reflns_used    8506
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.2950
_cell_measurement_theta_min      4.6660
_cell_volume                     1672.27(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_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     22.00  49.00   1.00    1.00    --    0.00 -99.00  60.00   27
  2  \w     14.00  43.00   1.00    1.00    --    0.00 -99.00-180.00   29
  3  \w   -103.00  -5.00   1.00    4.00    --  -60.50  77.00-150.00   98
  4  \w   -118.00 -93.00   1.00    4.00    --  -60.50 -94.00 -60.00   25
  5  \w     64.00 116.00   1.00    4.00    --   60.50-125.00 150.00   52
  6  \w    141.00 176.00   1.00   16.00    --  121.00 111.00 150.00   35
  7  \w     35.00  90.00   1.00   16.00    --  121.00 -37.00 120.00   55
  8  \w     77.00 130.00   1.00   16.00    --  121.00  77.00   0.00   53
  9  \w    101.00 127.00   1.00   16.00    --  121.00 111.00 150.00   26
 10  \w    145.00 173.00   1.00   16.00    --  121.00  77.00   0.00   28
 11  \w     45.00  83.00   1.00   16.00    --  121.00 -37.00  30.00   38
 12  \w     28.00  63.00   1.00   16.00    --  121.00 -25.00   0.00   35
 13  \w     32.00  94.00   1.00   16.00    --  121.00-111.00-180.00   62
 14  \w      1.00  26.00   1.00    1.00    --    0.00 -99.00  60.00   25
 15  \w      5.00  30.00   1.00    1.00    --    0.00-101.00-128.00   25
 16  \w   -154.00 -80.00   1.00    4.00    --  -60.50 -94.00-180.00   74
 17  \w      5.00  37.00   1.00    4.00    --   60.50  30.00-180.00   32
 18  \w    124.00 151.00   1.00    4.00    --   60.50 125.00  30.00   27
 19  \w    118.00 146.00   1.00    4.00    --   60.50  30.00-180.00   28
 20  \w     67.00 105.00   1.00   16.00    --  121.00 -50.00-150.00   38
 21  \w    120.00 146.00   1.00   16.00    --  121.00  37.00  90.00   26
 22  \w    137.00 164.00   1.00   16.00    --  121.00 -77.00-150.00   27
 23  \w     81.00 111.00   1.00   16.00    --  121.00-111.00  60.00   30
 24  \w     29.00  55.00   1.00   16.00    --  121.00-111.00  60.00   26
 25  \w     30.00  65.00   1.00   16.00    --  121.00 -37.00-150.00   35
 26  \w     34.00  88.00   1.00   16.00    --  121.00 -25.00-150.00   54
 27  \w     85.00 119.00   1.00   16.00    --  121.00 -77.00-150.00   34
 28  \w     21.00  48.00   1.00   16.00    --  121.00 -77.00-150.00   27
 29  \w      1.00  27.00   1.00    1.00    --    0.00 -99.00  90.00   26
 30  \w      2.00  28.00   1.00    1.00    --    0.00 -99.00 -90.00   26
 31  \w    -98.00 -73.00   1.00    4.00    --  -60.50-125.00 -30.00   25
 32  \w   -142.00-114.00   1.00    4.00    --  -60.50-125.00 -30.00   28
 33  \w   -143.00 -91.00   1.00    4.00    --  -60.50 -94.00 120.00   52
 34  \w    127.00 152.00   1.00    4.00    --   60.50 125.00  90.00   25
 35  \w    114.00 141.00   1.00    4.00    --   60.50 125.00 150.00   27
 36  \w    150.00 177.00   1.00   16.00    --  121.00  50.00-150.00   27
 37  \w    136.00 166.00   1.00   16.00    --  121.00 111.00 120.00   30
 38  \w    150.00 176.00   1.00   16.00    --  121.00 111.00  30.00   26
 39  \w     34.00  71.00   1.00   16.00    --  121.00 -37.00 -90.00   37
 40  \w    110.00 136.00   1.00   16.00    --  121.00  50.00-150.00   26
 41  \w    145.00 173.00   1.00   16.00    --  121.00 111.00-180.00   28
 42  \w    109.00 135.00   1.00   16.00    --  121.00  50.00 120.00   26
 43  \w     64.00  90.00   1.00    1.00    --    0.00  37.00-120.00   26
 44  \w    -34.00  -8.00   1.00    1.00    --    0.00  37.00-120.00   26
 45  \w     -4.00  23.00   1.00    1.00    --    0.00  37.00-120.00   27
 46  \w     -6.00  26.00   1.00    4.00    --  -60.50  30.00 -60.00   32
 47  \w    -48.00 -15.00   1.00    4.00    --  -60.50  30.00 -60.00   33
 48  \w   -146.00 -82.00   1.00    4.00    --  -60.50 -94.00 -90.00   64
 49  \w    -79.00 -53.00   1.00    4.00    --  -60.50 125.00 -30.00   26
 50  \w     35.00 120.00   1.00    4.00    --   60.50  30.00-180.00   85
 51  \w     96.00 122.00   1.00    4.00    --   60.50 125.00 120.00   26
 52  \w     61.00  87.00   1.00   16.00    --  121.00-111.00   0.00   26
 53  \w     79.00 105.00   1.00   16.00    --  121.00-111.00  90.00   26
 54  \w     50.00  76.00   1.00   16.00    --  121.00-111.00 -90.00   26
 55  \w     45.00 111.00   1.00   16.00    --  121.00-111.00-150.00   66
 56  \w    152.00 177.00   1.00   16.00    --  121.00 111.00  90.00   25
 57  \w     47.00 112.00   1.00   16.00    --  121.00-111.00 120.00   65
 58  \w     80.00 130.00   1.00   16.00    --  121.00  50.00 150.00   50
 59  \w     73.00 112.00   1.00   16.00    --  121.00-111.00  30.00   39
 60  \w     89.00 174.00   1.00   16.00    --  121.00 -12.00-180.00   85
 61  \w     32.00  68.00   1.00   16.00    --  121.00 -12.00-180.00   36
 62  \w     46.00 109.00   1.00   16.00    --  121.00-111.00 150.00   63
 63  \w     78.00 106.00   1.00   16.00    --  121.00-111.00 -30.00   28
 64  \w     46.00  72.00   1.00   16.00    --  121.00 -37.00-150.00   26
 65  \w    109.00 147.00   1.00   16.00    --  121.00 111.00-180.00   38
 66  \w     79.00 112.00   1.00   16.00    --  121.00-111.00 -90.00   33
 67  \w    141.00 166.00   1.00   16.00    --  121.00  50.00 150.00   25
 68  \w     60.00  86.00   1.00   16.00    --  121.00-111.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0830135000
_diffrn_orient_matrix_UB_12      -0.0758576000
_diffrn_orient_matrix_UB_13      0.0366261000
_diffrn_orient_matrix_UB_21      -0.0419119000
_diffrn_orient_matrix_UB_22      0.0094967000
_diffrn_orient_matrix_UB_23      -0.1524285000
_diffrn_orient_matrix_UB_31      0.0684564000
_diffrn_orient_matrix_UB_32      -0.0862975000
_diffrn_orient_matrix_UB_33      -0.0489514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         4.684
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+2.8250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1693
_reflns_number_total             1762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00235a2.cif
_cod_data_source_block           nabarf4
_cod_original_cell_volume        1672.27(7)
_cod_database_code               7049019
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C32 H12 B1 F24 Na1'
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.724
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6-F5 \\sim F6-F4 \\sim F5A-F4A \\sim F5A-F6A \\sim F5-F4 \\sim F4A-F6A
 with sigma of 0.02
 C8-F6 \\sim C8-F5A \\sim C8-F5 \\sim C8-F4A \\sim C8-F4 \\sim C8-F6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C8, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
;
_shelx_res_checksum              10726
_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 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.741