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_4111379
_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         'C38 H37 Sc Si2'
_chemical_formula_sum            'C38 H37 Sc Si2'
_chemical_formula_weight         594.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Dec 13 13:41:59 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90.000(1)
_cell_angle_beta                 95.289(1)
_cell_angle_gamma                90.000(1)
_cell_formula_units_Z            4
_cell_length_a                   9.9125(8)
_cell_length_b                   20.937(2)
_cell_length_c                   16.232(1)
_cell_measurement_reflns_used    4204
_cell_measurement_temperature    135.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      3.5
_cell_volume                     3354.4(5)
_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      135.2
_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  0.0435
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13104
_diffrn_reflns_theta_max         24.70
_diffrn_source                   'X-ray tube'
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             1256.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.455
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.9680
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0612
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                3349
_reflns_number_total             5548
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            ja040141r_s2.cif
_cod_data_source_block           Cp*2ScSiH2SiPh3
_cod_original_cell_volume        3354.3(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111379