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_4107206
_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         'C56 H90 Br2 Si2'
_chemical_formula_sum            'C56 H90 Br2 Si2'
_chemical_formula_weight         979.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.705(2)
_cell_angle_beta                 101.795(3)
_cell_angle_gamma                97.157(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9767(13)
_cell_length_b                   13.028(2)
_cell_length_c                   13.623(3)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    200
_cell_measurement_theta_max      32.5607
_cell_measurement_theta_min      2.4804
_cell_volume                     1342.1(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
        Number of images: 360
                   Slice: -70.0000 - 110.0000
             Image width: 0.5000
                Exp time: 1.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 50.0000
                     Phi: 270.0000
                     XTD: 40.0947
                  2theta: 20.0722
scan:
        Number of images: 360
                   Slice: -70.0000 - 110.0000
             Image width: 0.5000
                Exp time: 1.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 50.0000
                     Phi: 90.0000
                     XTD: 40.0947
                  2theta: 20.0722
scan:
        Number of images: 360
                   Slice: -70.0000 - 110.0000
             Image width: 0.5000
                Exp time: 1.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 50.0000
                     Phi: 45.0000
                     XTD: 40.0947
                  2theta: 20.0722
scan:
        Number of images: 360
                   Slice: -70.0000 - 110.0000
             Image width: 0.5000
                Exp time: 1.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 30.0000
                     Phi: 270.0000
                     XTD: 40.0947
                  2theta: 20.0722
scan:
        Number of images: 360
                   Slice: -70.0000 - 110.0000
             Image width: 0.5000
                Exp time: 1.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 0.0000
                     Phi: 0.0000
                     XTD: 40.0947
                  2theta: 20.0722
;
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.1221
_diffrn_orient_matrix_UB_12      -0.0310
_diffrn_orient_matrix_UB_13      0.0317
_diffrn_orient_matrix_UB_21      0.0037
_diffrn_orient_matrix_UB_22      -0.0788
_diffrn_orient_matrix_UB_23      -0.0079
_diffrn_orient_matrix_UB_31      0.0059
_diffrn_orient_matrix_UB_32      -0.0239
_diffrn_orient_matrix_UB_33      0.0728
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34822
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.48
_diffrn_source_current           24
_diffrn_source_power             1.2
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_T_max  0.8606
_exptl_absorpt_correction_T_min  0.6411
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numabs
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                5676
_reflns_number_total             7804
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja209736d_si_002.cif
_cod_data_source_block           Dibromodisilene
_cod_database_code               4107206