Alkali metal reduction of 2-halogeno- and 2-thiolato-2,3-dihydro-1H-1,3,2-diazaboroles
Weber, Lothar; Schnieder, Markus; Lönnecke, Peter; Journal of the Chemical Society, Dalton Transactions  (2001) 3459–; doi:10.1039/b106128n

data_7010980
_publ_section_title
;
 Alkali metal reduction of 2-halogeno- and
 2-thiolato-2,3-dihydro-1H-1,3,2-diazaboroles
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3459
_journal_paper_doi               10.1039/b106128n
_journal_year                    2001
_chemical_formula_sum            'C20 H28 B2 N4'
_chemical_formula_weight         346.08
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.582(5)
_cell_length_b                   6.952(2)
_cell_length_c                   15.511(5)
_cell_measurement_reflns_used    1766
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.19
_cell_volume                     2003.7(10)
_computing_cell_refinement       'SAINT (AXS-Bruker)'
_computing_data_collection       'SMART (AXS-Bruker)'
_computing_data_reduction        'SAINT (AXS-Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD-Diffractometer (AXS Bruker)'
_diffrn_measurement_method       'omega scans'
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11876
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9669
_exptl_absorpt_correction_T_min  0.9541
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0064(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.2932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                1766
_reflns_number_total             2430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106128n.txt
_cod_data_source_block           c840_fin
_cod_original_cell_volume        2003.8(10)
_cod_original_sg_symbol_H-M      'P bcn'
_cod_database_code               7010980