Synthesis and Reactions of a Stable 1,2-Diaryl-1,2-dibromodisilene: A Precursor for Substituted Disilenes and a 1,2-Diaryldisilyne
Takahiro Sasamori; Koji Hironaka; Yusuke Sugiyama; Nozomi Takagi; Shigeru Nagase; Yoshinobu Hosoi; Yukio Furukawa; Norihiro Tokitoh; Journal of the American Chemical Society 130 (2008) 13856–13857; doi:10.1021/ja8061002

data_4108525
_publ_section_title
;
 Synthesis and Reactions of a Stable 1,2-Diaryl-1,2-dibromodisilene: A
 Precursor for Substituted Disilenes and a 1,2-Diaryldisilyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13856
_journal_page_last               13857
_journal_paper_doi               10.1021/ja8061002
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C64 H143 Br Si16'
_chemical_formula_sum            'C64 H143 Br Si16'
_chemical_formula_weight         1442.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.4142(8)
_cell_angle_beta                 99.4484(8)
_cell_angle_gamma                96.362(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2621(3)
_cell_length_b                   18.6172(3)
_cell_length_c                   19.7599(3)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.01
_cell_volume                     4294.70(14)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38311
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         15867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                10773
_reflns_number_total             15867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8061002_si_003.cif
_cod_data_source_block           sibu
_cod_original_sg_symbol_Hall     '    -P 1'
_cod_database_code               4108525