Facile 1,2-Migration of a Methyl Group on a {Dimethoxy(methyl)silyl}tungsten Complex: Formation of a Base-Stabilized (Dimethoxysilylene)(methyl) Complex†
Suzuki, Eiji; Komuro, Takashi; Kanno, Yuto; Okazaki, Masaaki; Tobita, Hiromi; Organometallics 29 (2010) 5296–; doi:10.1021/om100399s

data_4066329
_publ_section_title
;
 Facile 1,2-Migration of a Methyl Group on a
 {Dimethoxy(methyl)silyl}tungsten Complex: Formation of a Base-Stabilized
 (Dimethoxysilylene)(methyl) Complex&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5296
_journal_paper_doi               10.1021/om100399s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C22 H34 N2 O4 Si W'
_chemical_formula_sum            'C22 H34 N2 O4 Si W'
_chemical_formula_weight         602.45
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 94.7457(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9831(4)
_cell_length_b                   16.8823(9)
_cell_length_c                   15.7119(10)
_cell_measurement_reflns_used    20340
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.2
_cell_volume                     2374.6(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP-3
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18997
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    4.945
_exptl_absorpt_correction_T_max  0.3712
_exptl_absorpt_correction_T_min  0.2171
_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            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+14.7977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                4894
_reflns_number_total             5405
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om100399s_si_002.cif
_cod_data_source_block           complex-cis3
_cod_database_code               4066329