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_4108524
_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         'C60 H134 Br2 Si16, 0.5(C6 H14)'
_chemical_formula_sum            'C63 H141 Br2 Si16'
_chemical_formula_weight         1508.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 101.5616(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5893(3)
_cell_length_b                   12.7057(2)
_cell_length_c                   38.2073(7)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.94
_cell_volume                     8841.1(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            72467
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.9440
_exptl_absorpt_correction_T_min  0.7211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       prism
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         15574
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0489P)^2^+9.5793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                11818
_reflns_number_total             15574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8061002_si_002.cif
_cod_data_source_block           thermo
_cod_original_sg_symbol_Hall     '    -P 2yn'
_cod_database_code               4108524