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_7047932
_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         'C28 H20 B O8, Li, (C6 H12 O2) 0.5(C6 H10 O)'
_chemical_formula_sum            'C37 H37 B Li O10.5'
_chemical_formula_weight         667.41
_chemical_melting_point          'decomposition > 190 C'
_chemical_name_systematic
;
Lithium tetrakis(3-carboxyphenyl)borate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.258(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1982(11)
_cell_length_b                   17.4686(5)
_cell_length_c                   17.705(2)
_cell_measurement_reflns_used    10533
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7980
_cell_measurement_theta_min      3.5780
_cell_volume                     4610.1(7)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
_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  51.00   1.00    5.00    --    0.00 -99.00  90.00   50
  2  \w    -42.00  92.00   1.00    5.00    --    0.00  57.00 -90.00  134
  3  \w    -96.00  -2.00   1.00   13.00    --  -60.50 125.00 -30.00   94
  4  \w   -156.00 -80.00   1.00   13.00    --  -60.50 -94.00 -90.00   76
  5  \w    -96.00  -2.00   1.00   13.00    --  -60.50 125.00 120.00   94
  6  \w     94.00 152.00   1.00   13.00    --   60.50 125.00  90.00   58
  7  \w     19.00 152.00   1.00   13.00    --   60.50  45.00 120.00  133
  8  \w     -4.00 109.00   1.00   13.00    --   60.50 -94.00  30.00  113
  9  \w     29.00 115.00   1.00   28.00    --  121.00-111.00   0.00   86
 10  \w     77.00 178.00   1.00   28.00    --  121.00  77.00 120.00  101
 11  \w    100.00 178.00   1.00   28.00    --  121.00 111.00   0.00   78
 12  \w     21.00 165.00   1.00   28.00    --  121.00 -77.00 150.00  144
 13  \w     77.00 178.00   1.00   28.00    --  121.00  63.00-120.00  101
 14  \w    100.00 178.00   1.00   28.00    --  121.00 111.00-150.00   78
 15  \w     29.00 115.00   1.00   28.00    --  121.00-111.00 -90.00   86
 16  \w     77.00 178.00   1.00   28.00    --  121.00  77.00 -90.00  101
 17  \w     29.00 115.00   1.00   28.00    --  121.00-111.00-150.00   86
 18  \w   -101.00 -35.00   1.00    5.00    --    0.00-178.00-180.00   66
 19  \w    -99.00 -34.00   1.00    5.00    --    0.00 178.00  30.00   65
 20  \w     18.00 153.00   1.00   13.00    --   60.50  61.00   0.00  135
;
_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      -0.0507841000
_diffrn_orient_matrix_UB_12      -0.0492922000
_diffrn_orient_matrix_UB_13      -0.0678766000
_diffrn_orient_matrix_UB_21      0.0537469000
_diffrn_orient_matrix_UB_22      -0.0723295000
_diffrn_orient_matrix_UB_23      0.0503175000
_diffrn_orient_matrix_UB_31      -0.1290374000
_diffrn_orient_matrix_UB_32      -0.0107065000
_diffrn_orient_matrix_UB_33      -0.0272217000
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33268
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.022
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colorless
_exptl_crystal_density_diffrn    0.962
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.765
_refine_ls_R_factor_all          0.1653
_refine_ls_R_factor_gt           0.1392
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_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          0.3900
_refine_ls_wR_factor_ref         0.4246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7059
_reflns_number_total             9580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04068k2.cif
_cod_data_source_block           4a_squeeze
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '__diffrn_orient_matrix_type' replaced with
'_diffrn_orient_matrix_type'.

Automatic conversion script
Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas 

 Adding full bibliography for 7047930--7047932.cif.
;
_cod_original_cell_volume        4610.0(7)
_cod_original_formula_sum        'C37 H37 B Li O10.50'
_cod_database_code               7047932
_oxdiff_exptl_absorpt_empirical_full_min 0.797
_oxdiff_exptl_absorpt_empirical_full_max 1.364
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4