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_4071484
_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 N2 O Os, C F3 O3 S'
_chemical_formula_sum            'C38 H51 F3 N2 O4 Os S'
_chemical_formula_weight         879.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 93.904(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   10.7729(15)
_cell_length_b                   22.084(3)
_cell_length_c                   16.445(2)
_cell_measurement_reflns_used    802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2.5
_cell_volume                     3903.3(9)
_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 0.992
_diffrn_measured_fraction_theta_max 0.910
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12492
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.374
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.819
_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 orange'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.768
_refine_diff_density_min         -2.767
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.043(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6641
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                5661
_reflns_number_total             6641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800183k-file001.cif
_cod_data_source_block           mae177as
_cod_original_cell_volume        3903.4(9)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4071484