Rhodium-catalysed synthesis of multi-substituted silylindenes from aryl alkynes and hydrosilanes via C-H bond activation
Shunsuke Sueki; Yoichiro Kuninobu; Chem.Commun. 51 (2015) 7685–; doi:10.1039/C5cc01569C

data_7117045
_publ_section_title
;
 Rhodium-catalysed synthesis of multi-substituted silylindenes from aryl
 alkynes and hydrosilanes via C-H bond activation
;
_journal_name_full               Chem.Commun.
_journal_page_first              7685
_journal_paper_doi               10.1039/C5cc01569C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C36 H32 Si'
_chemical_formula_sum            'C36 H32 Si'
_chemical_formula_weight         492.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-02-16 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.1822(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.0394(3)
_cell_length_b                   10.71244(19)
_cell_length_c                   18.6534(4)
_cell_measurement_reflns_used    20833
_cell_measurement_temperature    98
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.29
_cell_volume                     2680.20(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      98
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28254
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.00
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0713P)^2^+0.7774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                4275
_reflns_number_total             4890
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5cc01569c2.cif
_cod_data_source_block           3a
_cod_original_cell_volume        2680.19(9)
_cod_database_code               7117045