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_4071775
_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_sum            'C46 H41 B F4 Mo O4'
_chemical_formula_weight         840.54
_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                83.015(18)
_cell_angle_beta                 89.04(2)
_cell_angle_gamma                89.57(2)
_cell_formula_units_Z            4
_cell_length_a                   12.661(5)
_cell_length_b                   15.214(5)
_cell_length_c                   21.710(7)
_cell_measurement_reflns_used    3215
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4150(3)
_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    'SHELXS-97 (Sheldrick,1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.1843
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45230
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         0.94
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         16918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1707
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                7560
_reflns_number_total             16918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800379z_si_003.cif
_cod_data_source_block           mobf4-p-1
_cod_original_cell_volume        4150(2)
_cod_database_code               4071775