Borylene Insertion into Cage B-H Bond: A Route to Electron-Precise B-B Single Bond.
Wang, Hao; Zhang, Jiji; Lee, Hung Kay; Xie, Zuowei; Journal of the American Chemical Society 140 (2018) 3888–3891; doi:10.1021/jacs.8b01795

data_4132132
_publ_section_title
;
 Borylene Insertion into Cage B-H Bond: A Route to Electron-Precise B-B
 Single Bond.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3888
_journal_page_last               3891
_journal_paper_doi               10.1021/jacs.8b01795
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C49 H84 B11 Br N4 Na O2.5 Si2'
_chemical_formula_weight         1047.19
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2998(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0602(3)
_cell_length_b                   33.6570(8)
_cell_length_c                   15.0150(4)
_cell_measurement_reflns_used    158
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     6061.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo Diffractometer'
_diffrn_measurement_method       'Phi & Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66664
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7497
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10972
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+7.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2191
_reflns_number_gt                7628
_reflns_number_total             10972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b01795_si_003.cif
_cod_data_source_block           '[3Na]2'
_cod_depositor_comments
;

2024-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C98 H168 B22 Br2 N8 Na2 O5 Si4'
_cod_original_formula_weight         2094.38
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132132