Synthesis of tetraarylborates via tetralithio intermediates and the effect of polar functional groups and cations on their crystal structures.
Tomaszewski, Patryk; Wiszniewski, Marcin; Serwatowski, Janusz; Woźniak, Krzysztof; Durka, Krzysztof; Luliński, Sergiusz; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16627–16637; doi:10.1039/c8dt04068k

data_7047931
_publ_section_title
;
 Synthesis of tetraarylborates via tetralithio intermediates and the
 effect of polar functional groups and cations on their crystal
 structures.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16627
_journal_page_last               16637
_journal_paper_doi               10.1039/c8dt04068k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C44 H56 B N4 O4, Li, 3(C3H6O), 0.5 O'
_chemical_formula_sum            'C53 H74 B Li N4 O7.5'
_chemical_formula_weight         904.91
_chemical_melting_point          'decomposition > 280 C'
_chemical_name_systematic
;
 Lithium tetrakis[4-(N-tert-butylcarbamoyl)phenyl]borate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-09-19 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.517(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.560(3)
_cell_length_b                   22.0645(18)
_cell_length_c                   16.8909(18)
_cell_measurement_reflns_used    2062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.2150
_cell_measurement_theta_min      3.4330
_cell_volume                     5954.4(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.598
_diffrn_measured_fraction_theta_max 0.990
_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      1.00  82.00   1.00   20.00    --   31.40 -99.00 -90.00   81
  2  \w     57.00 133.00   1.00   20.00    --   31.40 178.00-180.00   76
  3  \w    -74.00  59.00   1.00   20.00    --  -32.65  57.00-120.00  133
  4  \w     94.00 161.00   1.00   55.00    --   69.05 125.00 -90.00   67
  5  \w     94.00 161.00   1.00   55.00    --   69.05 125.00  90.00   67
  6  \w   -166.00 -80.00   1.00   55.00    --  -70.30 -94.00 150.00   86
  7  \w    -84.00 -44.00   1.00   55.00    --  -70.30 -61.00-150.00   40
  8  \w   -125.00 -80.00   1.00   55.00    --  -70.30 -94.00-120.00   45
  9  \w   -162.00-122.00   1.00   55.00    --  -70.30 -61.00-150.00   40
 10  \w   -149.00 -80.00   1.00   55.00    --  -70.30 -94.00-180.00   69
 11  \w   -166.00-102.00   1.00   55.00    --  -70.30 -94.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0775738000
_diffrn_orient_matrix_UB_12      -0.0307393000
_diffrn_orient_matrix_UB_13      -0.0696485000
_diffrn_orient_matrix_UB_21      -0.0569636000
_diffrn_orient_matrix_UB_22      0.0372001000
_diffrn_orient_matrix_UB_23      0.0308605000
_diffrn_orient_matrix_UB_31      -0.0053645000
_diffrn_orient_matrix_UB_32      0.0504537000
_diffrn_orient_matrix_UB_33      -0.0651202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.1193
_diffrn_reflns_Laue_measured_fraction_full 0.598
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16879
_diffrn_reflns_point_group_measured_fraction_full 0.598
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.489
_diffrn_reflns_theta_min         2.766
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.99461
_exptl_absorpt_correction_T_min  0.99461
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         6449
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1956
_refine_ls_R_factor_gt           0.1089
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2856
_refine_ls_wR_factor_ref         0.3516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3116
_reflns_number_total             6449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04068k2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7047930--7047932.cif.'
_cod_original_cell_volume        5954.4(13)
_cod_original_formula_sum        'C53 H74 B Li N4 O7.50'
_cod_database_code               7047931
_oxdiff_exptl_absorpt_empirical_full_min 0.677
_oxdiff_exptl_absorpt_empirical_full_max 1.528
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4
_shelx_res_checksum              8886