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_4066328
_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         'C25 H40 N2 O2 Si W'
_chemical_formula_sum            'C25 H40 N2 O2 Si W'
_chemical_formula_weight         612.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   13.4319(2)
_cell_length_b                   28.3133(3)
_cell_length_c                   13.60540(10)
_cell_measurement_reflns_used    57560
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     5174.15(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39956
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    4.534
_exptl_absorpt_correction_T_max  0.6857
_exptl_absorpt_correction_T_min  0.6475
_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    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0317P)^2^+14.4367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                5091
_reflns_number_total             5908
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om100399s_si_002.cif
_cod_data_source_block           complex-2b
_cod_database_code               4066328