Insertion of carbon monoxide into an aldehyde CO double bond induced by an (η3-α-silabenzyl)carbonylmolybdenum complex
Kanno, Yuto; Komuro, Takashi; Tobita, Hiromi; RSC Adv. 4 (2014) 19068–; doi:10.1039/C4RA02308K

data_7235629
_publ_section_title
;
 Insertion of carbon monoxide into an aldehyde C&#xE001;O double bond
 induced by an (\h3-\a-silabenzyl)carbonylmolybdenum complex
;
_journal_issue                   37
_journal_name_full               'RSC Adv.'
_journal_page_first              19068
_journal_paper_doi               10.1039/C4RA02308K
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C37 H44 Mo O3 Si'
_chemical_formula_sum            'C37 H44 Mo O3 Si'
_chemical_formula_weight         660.75
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                95.4889(13)
_cell_angle_beta                 92.2032(14)
_cell_angle_gamma                97.1362(15)
_cell_formula_units_Z            4
_cell_length_a                   8.6566(3)
_cell_length_b                   10.9696(4)
_cell_length_c                   35.7255(11)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      69.61
_cell_measurement_theta_min      3.73
_cell_volume                     3346.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'Bruker D8 goniometer with CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            31297
_diffrn_reflns_theta_full        69.71
_diffrn_reflns_theta_max         69.71
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.806
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS (Sheldrick, 1996) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.863
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         11121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.361
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0000P)^2^+29.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                10971
_reflns_number_total             11121
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ra02308k2.cif
_cod_data_source_block           complex-2a
_cod_database_code               7235629