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_7049018
_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 K2)'
_chemical_formula_sum            'C32 H12 B F24 K'
_chemical_formula_weight         902.33
_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'
_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                   13.4834(3)
_cell_length_b                   13.4834(3)
_cell_length_c                   9.4747(5)
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      74.7320
_cell_measurement_theta_min      4.6120
_cell_volume                     1722.52(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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 0.992
_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    -47.00  30.00   1.00    1.00    --  -41.77  37.00 150.00   77
  2  \w     50.00  95.00   1.00    1.00    --   41.77-125.00 150.00   45
  3  \w     50.00 121.00   1.00    1.50    --  111.00-125.00 120.00   71
  4  \w     59.00  89.00   1.00    1.50    --  111.00 -30.00  90.00   30
  5  \w     41.00  68.00   1.00    1.50    --  111.00 -45.00  90.00   27
  6  \w     40.00  98.00   1.00    1.50    --  111.00 -45.00 -30.00   58
  7  \w     65.00  94.00   1.00    1.50    --  111.00-125.00 -60.00   29
  8  \w     38.00  85.00   1.00    1.50    --  111.00 -30.00 -90.00   47
  9  \w     44.00  88.00   1.00    1.50    --  111.00 -30.00-180.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0762435000
_diffrn_orient_matrix_UB_12      -0.0846036000
_diffrn_orient_matrix_UB_13      -0.0127627000
_diffrn_orient_matrix_UB_21      0.0023583000
_diffrn_orient_matrix_UB_22      0.0141804000
_diffrn_orient_matrix_UB_23      -0.1613759000
_diffrn_orient_matrix_UB_31      0.0849700000
_diffrn_orient_matrix_UB_32      0.0755153000
_diffrn_orient_matrix_UB_33      0.0158551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.811
_diffrn_reflns_theta_min         4.638
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
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    1.740
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1783
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0660P)^2^+2.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1554
_reflns_number_total             1783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00235a2.cif
_cod_data_source_block           kbarf4
_cod_original_cell_volume        1722.52(12)
_cod_database_code               7049018
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 B1 Co1 F24 N3 P2'
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.603
_reflns_odcompleteness_completeness 99.73
_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
 F2-F3 \\sim F2-F1 \\sim F2A-F3A \\sim F2A-F1A \\sim F3A-F1A \\sim F3-F1
 with sigma of 0.04
 F2-C7 \\sim F2A-C7 \\sim F1-C7 \\sim F1A-C7 \\sim F3-C7 \\sim F3A-C7
 with sigma of 0.02
 F5-F6 \\sim F4-F6 \\sim F4-F5 \\sim F6A-F5A \\sim F6A-F4A \\sim F5A-F4A
 with sigma of 0.04
 C8A-F6A \\sim C8A-F5A \\sim C8A-F4A \\sim C8-F6 \\sim C8-F4 \\sim C8-F5
 with sigma of 0.02
3. Restrained planarity
 C8A, C5, C4, C3, C2, C1, C6
 with sigma of 0.1
 C8, C5, C4, C3, C2, C1, C6
 with sigma of 0.1
4. Rigid bond restraints
 C8, F6, F4, F5, C8A, F6A, F5A, F4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
F2 \\sim F1 \\sim F3 \\sim C7 \\sim F3A \\sim F1A \\sim F2A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C8A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F5A \\sim F5 \\sim F6A \\sim F6 \\sim F4A \\sim F4: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C8A) = Uanis(C8)
6. Rigid body (RIGU) restrains
 F2, F1, F3, C7, F3A, F1A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F2)=Sof(F1)=Sof(F3)=FVAR(1)
 Sof(C8A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(2)
 Sof(C8)=Sof(F6)=Sof(F4)=Sof(F5)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4)
;
_shelx_res_checksum              54308
_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 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.904