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_4086092
_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 H34 Mo N2 O2 Si'
_chemical_formula_sum            'C31 H34 Mo N2 O2 Si'
_chemical_formula_weight         590.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.028(3)
_cell_angle_beta                 89.2027(15)
_cell_angle_gamma                88.1252(19)
_cell_formula_units_Z            4
_cell_length_a                   8.6869(3)
_cell_length_b                   18.5852(3)
_cell_length_c                   19.3204(2)
_cell_measurement_reflns_used    38490
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.2
_cell_volume                     2802.72(13)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37898
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.920175
_exptl_absorpt_correction_T_min  0.872027
_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    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         3.013
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0740P)^2^+20.0078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                10926
_reflns_number_total             12348
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00335_si_002.cif
_cod_data_source_block           complex-3
_cod_depositor_comments
'Adding full bibliography for 4086090--4086094.cif.'
_cod_original_cell_volume        2802.72(11)
_cod_database_code               4086092