Isolation and Reactivity of 1,4,2-Diazaborole.
Su, Bochao; Li, Yongxin; Ganguly, Rakesh; Lim, Jenny; Kinjo, Rei; Journal of the American Chemical Society 137 (2015) 11274–11277; doi:10.1021/jacs.5b07823

data_4124612
_publ_section_title
;
 Isolation and Reactivity of 1,4,2-Diazaborole.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11274
_journal_page_last               11277
_journal_paper_doi               10.1021/jacs.5b07823
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C39.5 H55.5 B Cl2.25 N4.75'
_chemical_formula_weight         687.46
_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
_cell_angle_alpha                90
_cell_angle_beta                 111.7249(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0389(4)
_cell_length_b                   31.4758(13)
_cell_length_c                   12.8082(5)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    153.(2)
_cell_measurement_theta_max      29.9115
_cell_measurement_theta_min      2.3131
_cell_volume                     3759.7(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2014)'
_diffrn_ambient_temperature      153.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60363
_diffrn_reflns_theta_full        31.08
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         12017
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+2.7137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                9128
_reflns_number_total             12017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07823_si_002.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C39.50 H55.50 B Cl2.25 N4.75'
_cod_database_code               4124612
_shelx_res_checksum              2697
_shelx_hkl_checksum              32633