Imine chloroboration: reaction of boron trichloride with a bulky diazadiene gives not a diazaborolium salt, but a 2,4,5-trichloro-1,3,2-diazaborolidine
Mair, Francis S.; Manning, Robert; Pritchard, Robin G.; Warren, John E.; Chemical Communications  (2001) 1136–; doi:10.1039/b101580j

data_7114883
_publ_section_title
;
 Imine chloroboration: reaction of boron trichloride with a bulky
 diazadiene gives not a diazaborolium salt, but a
 2,4,5-trichloro-1,3,2-diazaborolidine
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1136
_journal_paper_doi               10.1039/b101580j
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H36 B1 N2 Cl3'
_chemical_formula_structural     'C26 H36 B1 N2 CL3'
_chemical_formula_sum            'C26 H36 B Cl3 N2'
_chemical_formula_weight         493.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
;
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
;
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-04-04T10:18:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.246(3)
_cell_angle_beta                 90.208(2)
_cell_angle_gamma                115.0350(10)
_cell_formula_units_Z            2
_cell_length_a                   8.323(4)
_cell_length_b                   9.8086(3)
_cell_length_c                   17.35350(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1280.9(6)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.38482E-1
_diffrn_orient_matrix_UB_12      0.1108
_diffrn_orient_matrix_UB_13      -0.3406E-2
_diffrn_orient_matrix_UB_21      -0.125594
_diffrn_orient_matrix_UB_22      -0.18105E-1
_diffrn_orient_matrix_UB_23      -0.11268E-1
_diffrn_orient_matrix_UB_31      -0.18582E-1
_diffrn_orient_matrix_UB_32      0.01046
_diffrn_orient_matrix_UB_33      0.56532E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4812
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.3
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   7
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.28
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.3057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                3324
_reflns_number_total             4475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101580j.txt
_cod_data_source_block           c
_cod_original_cell_volume        1281.0(6)
_cod_database_code               7114883
_exptl_absorpt_factor_mur        0.047
_exptl_absorpt_correction_t_ave  0.9236
_diffrn_standards_decay_corr_max 1.056
_diffrn_standards_decay_corr_min 0.903