(η3-α-Silabenzyl)tungsten Complexes: An Isolable Intermediate for Interconversion between a Silylene Complex and a Silyl Complex through 1,2-Aryl Migration
Suzuki, Eiji; Komuro, Takashi; Kanno, Yuto; Tobita, Hiromi; Organometallics 32 (2013) 748–; doi:10.1021/om4000105

data_4080056
_publ_section_title
;
 (\h3-\a-Silabenzyl)tungsten Complexes: An Isolable Intermediate for
 Interconversion between a Silylene Complex and a Silyl Complex through
 1,2-Aryl Migration
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              748
_journal_paper_doi               10.1021/om4000105
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C33 H36 O2 Si W'
_chemical_formula_sum            'C33 H36 O2 Si W'
_chemical_formula_weight         676.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.2999(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.42620(10)
_cell_length_b                   32.5783(3)
_cell_length_c                   10.41630(10)
_cell_measurement_reflns_used    48709
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.2
_cell_volume                     2857.09(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material
; 
'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27400
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    4.113
_exptl_absorpt_correction_T_max  0.544385
_exptl_absorpt_correction_T_min  0.441141
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan. 
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+5.3819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                5903
_reflns_number_total             6400
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4000105_si_002.cif
_cod_data_source_block           complex-1b
_cod_database_code               4080056