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_4107207
_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         'C33 H49 Br N2 Si, C6 H6'
_chemical_formula_sum            'C39 H55 Br N2 Si'
_chemical_formula_weight         659.85
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.547(3)
_cell_length_b                   12.5450(19)
_cell_length_c                   14.345(2)
_cell_measurement_reflns_used    9201
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3517.6(9)
_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      153
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-10 with Saturn724+'
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27543
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 REQAB implimented in the CrystalClear program.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7973
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                6258
_reflns_number_total             7973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja209736d_si_003.cif
_cod_data_source_block           Si-PPy
_cod_original_cell_volume        3517.7(9)
_cod_database_code               4107207