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_4108526
_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 Si16, 2(C7 H8)'
_chemical_formula_sum            'C74 H150 Si16'
_chemical_formula_weight         1489.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           94
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      94
_symmetry_space_group_name_Hall  'P 4n 2n'
_symmetry_space_group_name_H-M   'P 42 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6701(4)
_cell_length_b                   16.6701(4)
_cell_length_c                   33.7498(11)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.41
_cell_volume                     9378.8(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1966
_diffrn_reflns_av_sigmaI/netI    0.1538
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            70378
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_description       prism
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(3)
_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     446
_refine_ls_number_reflns         8253
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.2028
_reflns_number_gt                3799
_reflns_number_total             8253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8061002_si_004.cif
_cod_data_source_block           sisi
_cod_database_code               4108526