Room-Temperature Dissociation of 1,2-Dibromodisilenes to Bromosilylenes
Katsunori Suzuki; Tsukasa Matsuo; Daisuke Hashizume; Kohei Tamao; Journal of the American Chemical Society 133 (2011) 19710–19713; doi:10.1021/ja209736d

data_4107208
_publ_section_title
;
 Room-Temperature Dissociation of 1,2-Dibromodisilenes to Bromosilylenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19710
_journal_page_last               19713
_journal_paper_doi               10.1021/ja209736d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H55 Br Si3'
_chemical_formula_sum            'C32 H55 Br Si3'
_chemical_formula_weight         603.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 98.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.785(3)
_cell_length_b                   12.4724(15)
_cell_length_c                   25.669(3)
_cell_measurement_reflns_used    12699
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.4894
_cell_measurement_theta_min      3.0639
_cell_volume                     6894.4(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku AFC-10 whth Saturn724+ CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54850
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.8797
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 REQAB implemented in the CrystalClear program.

;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         15432
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0842P)^2^+3.2921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                9819
_reflns_number_total             15432
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja209736d_si_004.cif
_cod_data_source_block           Si-TMSCCTMS
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4107208