Half-Sandwich Complexes of Osmium(II) withl-α-Amino Carboxylate Ligands as Asymmetric Transfer Hydrogenation Catalysts. On the Origin of the Enantioselectivity
Carmona, Daniel; Lahoz, Fernando J.; García-Orduña, Pilar; Oro, Luis A.; Lamata, M. Pilar; Viguri, Fernando; Organometallics 31 (2012) 3333–; doi:10.1021/om3001394

data_4078145
_publ_section_title
;
 Half-Sandwich Complexes of Osmium(II) withl-\a-Amino Carboxylate Ligands
 as Asymmetric Transfer Hydrogenation Catalysts. On the Origin of the
 Enantioselectivity
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3333
_journal_paper_doi               10.1021/om3001394
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'(C48 H72 N3 O6 Os3 3+), 3 (B F4 1-), C4 H10 O'
_chemical_formula_sum            'C52 H82 B3 F12 N3 O7 Os3'
_chemical_formula_weight         1692.24
_chemical_name_systematic        ?
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.430(2)
_cell_length_b                   15.430(2)
_cell_length_c                   58.650(12)
_cell_measurement_reflns_used    4923
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.963
_cell_measurement_theta_min      2.138
_cell_volume                     13964(4)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1420
_diffrn_reflns_av_sigmaI/netI    0.1827
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            76838
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.521
_exptl_absorpt_correction_T_max  0.69509
_exptl_absorpt_correction_T_min  0.42905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.01.   
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6576
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.562
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12304
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                7192
_reflns_number_total             12304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3001394_si_001.cif
_cod_data_source_block           compnd_13
_cod_original_cell_volume        13965(4)
_cod_original_sg_symbol_H-M      P43212
_cod_database_code               4078145