Ionic Hydrogenation of Ketones with Molybdenum Pentabenzylcyclopentadienyl Hydride Catalysts
Namorado, Sónia; Antunes, Maria Augusta; Veiros, Luis F.; Ascenso, José R.; Duarte, M. Teresa; Martins, Ana M.; Organometallics 27 (2008) 4589–4599; doi:10.1021/om800379z

data_4071773
_publ_section_title
;
 Ionic Hydrogenation of Ketones with Molybdenum
 Pentabenzylcyclopentadienyl Hydride Catalysts
;
_journal_coden_ASTM              ORGND7
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4589
_journal_page_last               4599
_journal_paper_doi               10.1021/om800379z
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C44 H35 F3 Mo O6 S, 0.125 (C4 H10 O)'
_chemical_formula_sum            'C44.5 H36.25 F3 Mo O6.12 S'
_chemical_formula_weight         854.01
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.102(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0960(19)
_cell_length_b                   17.894(4)
_cell_length_c                   22.843(5)
_cell_measurement_reflns_used    6841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4085.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'ORTEP3 (J. Appl. Crystallogr. 1997, 30, 565)'
_computing_publication_material  'CIFTAB (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (J. Appl. Cryst. 1999, 32, 115-119)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85319
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.9381
_exptl_absorpt_correction_T_min  0.8463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9803
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.574
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1253P)^2^+6.0645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2068
_reflns_number_gt                7613
_reflns_number_total             9803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800379z_si_001.cif
_cod_data_source_block           sn176-p21c
_cod_original_cell_volume        4085.6(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44.50 H36.25 F3 Mo O6.12 S'
_cod_database_code               4071773