Si-H Bond Activation of Alkynylsilanes by Group 4 Metallocene Complexes
Martin Lamač; Anke Spannenberg; Wolfgang Baumann; Haijun Jiao; Christine Fischer; Sven Hansen; Perdita Arndt; Uwe Rosenthal; Journal of the American Chemical Society 132 (2010) 4369–4380; doi:10.1021/ja910527w

data_4102171
_publ_section_title
;
 Si-H Bond Activation of Alkynylsilanes by Group 4 Metallocene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4369
_journal_page_last               4380
_journal_paper_doi               10.1021/ja910527w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C28 H32 Si2 Ti'
_chemical_formula_weight         472.62
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.324(4)
_cell_angle_beta                 101.046(3)
_cell_angle_gamma                114.318(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5394(4)
_cell_length_b                   10.3251(5)
_cell_length_c                   16.5699(8)
_cell_measurement_reflns_used    5474
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.15
_cell_volume                     1287.09(11)
_computing_cell_refinement       'IPDS Program Package'
_computing_data_collection       'IPDS Program Package (Stoe & Cie, 2005)'
_computing_data_reduction        'IPDS Program Package'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24788
_diffrn_reflns_theta_full        29.23
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.8086
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6939
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                4795
_reflns_number_total             6939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910527w_si_002.cif
_cod_data_source_block           ks989
_cod_database_code               4102171