Synthesis and Characterization of Scandium Silyl Complexes of the Type Cp*2ScSiHRR'. σ-Bond Metathesis Reactions and Catalytic Dehydrogenative Silation of Hydrocarbons
Aaron D. Sadow; T. Don Tilley; Journal of the American Chemical Society 127 (2005) 643–656; doi:10.1021/ja040141r

data_4111378
_publ_contact_author_address
;
    Department of Chemistry
    University of California, Berkeley
    Berkeley, CA 94720-1460
;
_publ_contact_author_email       ' tdtilley@socrates.berkeley.edu '
_publ_contact_author_fax         ' 510 642 8940 '
_publ_contact_author_name        ' T. D. Tilley'
_publ_contact_author_phone       ' 510 642 1871 '
_publ_section_title
;
 Synthesis and Characterization of Scandium Silyl Complexes of the Type
 Cp*2ScSiHRR'. \s-Bond Metathesis Reactions and Catalytic Dehydrogenative
 Silation of Hydrocarbons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              643
_journal_page_last               656
_journal_paper_doi               10.1021/ja040141r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C26 H49 Sc Si3'
_chemical_formula_sum            'C26 H49 Sc Si3'
_chemical_formula_weight         490.89
_chemical_name_common            Cp*2ScSiH(SiMe3)2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Jun 11 06:53:12 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                94.074(1)
_cell_angle_beta                 105.507(1)
_cell_angle_gamma                103.560(1)
_cell_formula_units_Z            2
_cell_length_a                   9.1426(6)
_cell_length_b                   10.4602(6)
_cell_length_c                   17.096(1)
_cell_measurement_reflns_used    4330
_cell_measurement_temperature    132.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      3.5
_cell_volume                     1515.83(16)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      132.2
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7647
_diffrn_reflns_theta_max         24.68
_diffrn_source                   'X-ray tube'
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       blocks
_exptl_crystal_F_000             536.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.58
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.390
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0959
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                3756
_reflns_number_total             4799
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            ja040141r_s1.cif
_cod_data_source_block           Cp*2ScSiH(SiMe3)2
_cod_original_cell_volume        1515.9(2)
_cod_database_code               4111378