Direct Conversion of a Si‒C(aryl) Bond to Si‒Heteroatom Bonds in the Reactions of η3-α-Silabenzyl Molybdenum and Tungsten Complexes with 2-Substituted Pyridines
Kanno, Yuto; Komuro, Takashi; Tobita, Hiromi; Organometallics 34 (2015) 3699–; doi:10.1021/acs.organomet.5b00335

data_4086093
_publ_section_title
;
 Direct Conversion of a Si--C(aryl) Bond to Si--Heteroatom Bonds in the
 Reactions of \h3-\a-Silabenzyl Molybdenum and Tungsten Complexes with
 2-Substituted Pyridines
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3699
_journal_paper_doi               10.1021/acs.organomet.5b00335
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H33 N O2 S Si W'
_chemical_formula_sum            'C31 H33 N O2 S Si W'
_chemical_formula_weight         695.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 108.0170(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1899(6)
_cell_length_b                   9.3453(4)
_cell_length_c                   19.8995(9)
_cell_measurement_reflns_used    54723
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.3
_cell_volume                     2863.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics
;
'ORTEP-3', 'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)'
;
_computing_publication_material
;
'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39346
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    4.178
_exptl_absorpt_correction_T_max  0.595914
_exptl_absorpt_correction_T_min  0.374563
_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            dark-red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.404
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0576P)^2^+4.2871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                5979
_reflns_number_total             6552
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00335_si_002.cif
_cod_data_source_block           complex-4
_cod_depositor_comments
'Adding full bibliography for 4086090--4086094.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4086093