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_4106890
_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         'C46 H70 N2 O3 Si2 W1'
_chemical_formula_sum            'C46 H70 N2 O3 Si2 W'
_chemical_formula_weight         939.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0736(7)
_cell_length_b                   16.1627(8)
_cell_length_c                   20.5702(10)
_cell_measurement_reflns_used    26824
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      1.26
_cell_volume                     4664.1(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000), SORTAV'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku RAXIS-IV imaging plate'
_diffrn_measurement_method       dtintegrate.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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45453
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.424
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         11266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.424
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0064P)^2^+24.1136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                11124
_reflns_number_total             11266
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja207395w_si_002.cif
_cod_data_source_block           2.1hexane
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4106890