Synthesis, Structure, and Reactions of a (η3-α-silabenzyl)molybdenum Complex: A Synthetic Equivalent of a Coordinatively Unsaturated Silyl Complex
Komuro, Takashi; Kanno, Yuto; Tobita, Hiromi; Organometallics 32 (2013) 2795–; doi:10.1021/om400225j

data_4080826
_publ_section_title
;
 Synthesis, Structure, and Reactions of a (\h3-\a-silabenzyl)molybdenum
 Complex: A Synthetic Equivalent of a Coordinatively Unsaturated Silyl
 Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2795
_journal_paper_doi               10.1021/om400225j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C40 H46 Mo N2 O2 Si, 1.5(C4 H8 O)'
_chemical_formula_sum            'C46 H58 Mo N2 O3.5 Si'
_chemical_formula_weight         818.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.6454(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.6607(10)
_cell_length_b                   20.3913(7)
_cell_length_c                   20.7670(9)
_cell_measurement_reflns_used    23463
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.4
_cell_volume                     8569.0(6)
_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    'DIRDIF-99 (PATTY)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.958
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.956016
_exptl_absorpt_correction_T_min  0.871692
_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    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         9369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0929P)^2^+11.7407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                7565
_reflns_number_total             9369
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400225j_si_002.cif
_cod_data_source_block           complex-2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C46 H58 Mo N2 O3.50 Si'
_cod_database_code               4080826