Reduction and C(sp2)−H Bond Activation of Ketones Promoted by a Cyclopentadienyl-Osmium- Dihydride-Dihydrogen Complex
Esteruelas, Miguel A.; Hernández, Yohar A.; López, Ana M.; Oliván, Montserrat; Oñate, Enrique; Organometallics 24 (2005) 5989–; doi:10.1021/om0508177

data_4076209
_publ_section_title
;
 Reduction and C(sp2)&#x2212;H Bond Activation of Ketones Promoted by a
 Cyclopentadienyl-Osmium- Dihydride-Dihydrogen Complex
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5989
_journal_paper_doi               10.1021/om0508177
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C22 H34 B F4 O Os P'
_chemical_formula_weight         622.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                78.686(2)
_cell_angle_beta                 82.2820(10)
_cell_angle_gamma                78.1240(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9899(8)
_cell_length_b                   11.2125(10)
_cell_length_c                   11.9126(11)
_cell_measurement_reflns_used    4001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1146.71(18)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12019
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.674
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
 method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
  
 SADABS: Area-Detector Absorption Correction. Bruker-AXS 
  within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.948
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                4677
_reflns_number_total             5414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0508177si20050921_011252.cif
_cod_data_source_block           mae153as
_cod_database_code               4076209