From Borapyramidane to Borole Dianion.
Lee, Vladimir Ya; Sugasawa, Haruka; Gapurenko, Olga A.; Minyaev, Ruslan M.; Minkin, Vladimir I.; Gornitzka, Heinz; Sekiguchi, Akira; Journal of the American Chemical Society 140 (2018) 6053–6056; doi:10.1021/jacs.8b03473

data_4132373
_publ_section_title
;
 From Borapyramidane to Borole Dianion.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6053
_journal_page_last               6056
_journal_paper_doi               10.1021/jacs.8b03473
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C24 H52 B Cl Li2 O2 Si4'
_chemical_formula_weight         545.15
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 103.570(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2197(15)
_cell_length_b                   20.178(3)
_cell_length_c                   18.246(3)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.27
_cell_volume                     3299.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31710
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.421
_diffrn_reflns_theta_min         1.529
_diffrn_source                   'Incoatec ImS'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9533
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+3.2442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4934
_reflns_number_total             6272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03473_si_004.cif
_cod_data_source_block           Diborole_0m
_cod_original_cell_volume        3299.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132373
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2014-3
_shelx_res_checksum              40720
_shelx_hkl_checksum              33820