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_4102174
_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            'C38 H38 Hf Si4'
_chemical_formula_weight         785.53
_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                88.056(2)
_cell_angle_beta                 84.173(2)
_cell_angle_gamma                80.283(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1828(2)
_cell_length_b                   10.4511(3)
_cell_length_c                   20.5913(6)
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      1.96
_cell_volume                     1726.47(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26806
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.186
_exptl_absorpt_correction_T_max  0.9264
_exptl_absorpt_correction_T_min  0.5197
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                6175
_reflns_number_total             7322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910527w_si_005.cif
_cod_data_source_block           ks1026
_cod_original_cell_volume        1726.47(9)
_cod_database_code               4102174