A Hypervalent Pentacoordinate Boron Compound with an N-B-N Three-Center Four-Electron Bond
Yuichi Hirano; Satoshi Kojima; Yohsuke Yamamoto; Journal of Organic Chemistry 76 (2011) 2123–2131; doi:10.1021/jo1024656

data_4026163
_publ_contact_author             'Dr. Satoshi Kojima'
_publ_contact_author_email       skojima@sci.hiroshima-u.ac.jp
_publ_section_title
;
 A Hypervalent Pentacoordinate Boron Compound with an N-B-N Three-Center
 Four-Electron Bond
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2123
_journal_page_last               2131
_journal_paper_doi               10.1021/jo1024656
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C6 H2 Br Cl I2'
_chemical_formula_weight         443.24
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.429(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.1459(5)
_cell_length_b                   14.1723(16)
_cell_length_c                   15.5670(17)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.785
_cell_measurement_theta_min      3.160
_cell_volume                     914.38(18)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_source         'long-fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9381
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    11.465
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'ABSCOR (Higashi, 1995)'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.220
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4175
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                3743
_reflns_number_total             4175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1024656_si_001.cif
_cod_data_source_block           yh713
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4026163