Preparation, X-ray Structure, and Reactivity of an Osmium-Hydroxo Complex Stabilized by an N-Heterocyclic Carbene Ligand: A Base-Free Catalytic Precursor for Hydrogen Transfer from 2-Propanol to Aldehydes
Castarlenas, Ricardo; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 27 (2008) 3240–; doi:10.1021/om800183k

data_4071485
_publ_section_title
;
 Preparation, X-ray Structure, and Reactivity of an Osmium-Hydroxo Complex
 Stabilized by an N-Heterocyclic Carbene Ligand: A Base-Free Catalytic
 Precursor for Hydrogen Transfer from 2-Propanol to Aldehydes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3240
_journal_paper_doi               10.1021/om800183k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C37 H51 Cl N2 Os '
_chemical_formula_sum            'C37 H51 Cl N2 Os'
_chemical_formula_weight         749.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.684(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.127(3)
_cell_length_b                   12.312(3)
_cell_length_c                   18.753(4)
_cell_measurement_reflns_used    902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      2
_cell_volume                     3383.3(13)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21929
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.499
_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.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.026
_refine_diff_density_min         -2.438
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5956
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                4377
_reflns_number_total             5956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800183k-file001.cif
_cod_data_source_block           mae227as
_cod_original_cell_volume        3383.3(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071485