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_4078144
_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
'C45 H66 N3 O3 Os3,3(B F4), 0.5(C4 H10 O),C H4 O'
_chemical_formula_sum            'C48 H75 B3 F12 N3 O7.5 Os3'
_chemical_formula_weight         1645.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   15.016(16)
_cell_length_b                   19.85(2)
_cell_length_c                   20.50(2)
_cell_measurement_reflns_used    1804
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.21
_cell_measurement_theta_min      2.235
_cell_volume                     6110(11)
_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 0.983
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker SMART APEX CCD sysyem'
_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  0.1283
_diffrn_reflns_av_sigmaI/netI    0.3736
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29688
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    6.305
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         13299
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                4479
_reflns_number_total             13299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3001394_si_001.cif
_cod_data_source_block           compnd_12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6112(11)
_cod_original_formula_sum        'C48 H75 B3 F12 N3 O7.50 Os3'
_cod_database_code               4078144