Synthesis and Characterization of κ2C,N-N-Silyliminoacyl Tungsten Complexes Cp*(CO)2W{κ2C,N-C(R)═NSiR′3} [R = Me, Et,i-Pr,t-Bu; R′3= (p-Tol)2Me, (p-Tol)3, Et3; Cp* = η5-C5Me5]: Thermally Induced Carbon−Carbon Bond Cleavage of Their Iminoacyl Ligands
Suzuki, Eiji; Komuro, Takashi; Kanno, Yuto; Okazaki, Masaaki; Tobita, Hiromi; Organometallics 29 (2010) 1839–; doi:10.1021/om901123w

data_4067776
_publ_section_title
;
 Synthesis and Characterization of \k2C,N-N-Silyliminoacyl Tungsten
 Complexes Cp*(CO)2W{\k2C,N-C(R)&#x2550;NSiR&#x2032;3} [R = Me,
 Et,i-Pr,t-Bu; R&#x2032;3= (p-Tol)2Me, (p-Tol)3, Et3; Cp* = \h5-C5Me5]:
 Thermally Induced Carbon&#x2212;Carbon Bond Cleavage of Their Iminoacyl
 Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1839
_journal_paper_doi               10.1021/om901123w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C36 H41 N O2 Si W'
_chemical_formula_sum            'C36 H41 N O2 Si W'
_chemical_formula_weight         731.64
_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                 91.9946(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0675(3)
_cell_length_b                   14.7448(4)
_cell_length_c                   24.3446(8)
_cell_measurement_reflns_used    33501
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     3252.86(18)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  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 0.963
_diffrn_measured_fraction_theta_max 0.946
_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  0.1280
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26148
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.619
_exptl_absorpt_correction_T_max  0.4098
_exptl_absorpt_correction_T_min  0.3254
_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            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.843
_refine_diff_density_min         -3.164
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0858P)^2^+7.9429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                6294
_reflns_number_total             7063
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om901123w_si_002.cif
_cod_data_source_block           complex3b
_cod_database_code               4067776