Access to B=S and B=Se Double Bonds via Sulfur and Selenium Insertion into a B-H Bond and Hydrogen Migration
Hao Wang; Jianying Zhang; Hongfan Hu; Chunming Cui; Journal of the American Chemical Society 132 (2010) 10998–10999; doi:10.1021/ja105021d

data_4102847
_publ_section_title
;
 Access to B=S and B=Se Double Bonds via Sulfur and Selenium Insertion
 into a B-H Bond and Hydrogen Migration
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10998
_journal_page_last               10999
_journal_paper_doi               10.1021/ja105021d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C21 H25 B N2 S, 2(C4 H8 O)'
_chemical_formula_sum            'C29 H41 B N2 O2 S'
_chemical_formula_weight         492.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.602(3)
_cell_length_b                   14.663(3)
_cell_length_c                   14.029(3)
_cell_measurement_reflns_used    6632
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      3.41
_cell_volume                     2787.3(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.6
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Saturn 724CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21854
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         21854
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+4.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2611
_refine_ls_wR_factor_ref         0.2708
_reflns_number_gt                20012
_reflns_number_total             21854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105021d_si_002.cif
_cod_data_source_block           hklf5
_cod_original_cell_volume        2787.5(10)
_cod_database_code               4102847