Reactions of Hydrido(hydrosilylene)tungsten Complexes with α,β-Unsaturated Carbonyl Compounds: Selective Formation of (η3-Siloxyallyl)tungsten Complexes
Takahito Watanabe; Hisako Hashimoto; Hiromi Tobita; Journal of the American Chemical Society 129 (2007) 11338–11339; doi:10.1021/ja074629e

data_4109949
_publ_contact_author_address
;
    ENTER CONTACT AUTHOR ADDRESS
;
_publ_contact_author_email       hhashimoto@mail.tains.tohoku.ac.jp
_publ_contact_author_name        'Hisako Hashimoto'
_publ_section_title
;
 Reactions of Hydrido(hydrosilylene)tungsten Complexes with
 \a,\b-Unsaturated Carbonyl Compounds: Selective Formation of
 (\h3-Siloxyallyl)tungsten Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11338
_journal_page_last               11339
_journal_paper_doi               10.1021/ja074629e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C27 H52 O3 Si4 W'
_chemical_formula_sum            'C27 H52 O3 Si4 W'
_chemical_formula_weight         720.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8869(4)
_cell_length_b                   8.9296(4)
_cell_length_c                   26.3746(8)
_cell_measurement_reflns_used    41979
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.77
_cell_volume                     3270.6(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29695
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_T_max  0.8365
_exptl_absorpt_correction_T_min  0.4237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6991
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+3.6978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                6474
_reflns_number_total             6991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074629esi20070709_104555.cif
_cod_data_source_block           complex2b
_cod_database_code               4109949