Synthesis of a Base-Stabilized Silanone-Coordinated Complex by Oxygenation of a (Silyl)(silylene)tungsten Complex
Takako Muraoka; Keisuke Abe; Youhei Haga; Tomoko Nakamura; Keiji Ueno; Journal of the American Chemical Society 133 (2011) 15365–15367; doi:10.1021/ja207395w

data_4106891
_publ_section_title
;
 Synthesis of a Base-Stabilized Silanone-Coordinated Complex by
 Oxygenation of a (Silyl)(silylene)tungsten Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15365
_journal_page_last               15367
_journal_paper_doi               10.1021/ja207395w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H48 O4 Si2 W1'
_chemical_formula_sum            'C32 H48 O4 Si2 W'
_chemical_formula_weight         736.73
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.318(17)
_cell_angle_beta                 83.570(18)
_cell_angle_gamma                80.960(18)
_cell_formula_units_Z            2
_cell_length_a                   11.414(2)
_cell_length_b                   12.2453(19)
_cell_length_c                   12.606(2)
_cell_measurement_reflns_used    477
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5754
_cell_measurement_theta_min      1.6555
_cell_volume                     1698.1(5)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.718
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17121
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         32.35
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    3.504
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8328
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       Block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.994
_refine_diff_density_min         -3.342
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+6.8350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                8623
_reflns_number_total             8694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207395w_si_003.cif
_cod_data_source_block           3'
_cod_original_cell_volume        1698.0(5)
_cod_database_code               4106891