Oxidation Catalysis of Nb(salan) Complexes: Asymmetric Epoxidation of Allylic Alcohols Using Aqueous Hydrogen Peroxide as an Oxidant
Hiromichi Egami; Takuya Oguma; Tsutomu Katsuki; Journal of the American Chemical Society 132 (2010) 5886–5895; doi:10.1021/ja100795k

data_4102323
_publ_contact_author_address
;

    Department of Chemistry
    Faculty of Science
    Kyushu University
    Hakozaki 6-10-1, Higashi-ku
    Fukuoka 812-8581, Japan
;
_publ_contact_author_email       katsuscc@mbox.nc.kyushu-u.ac.jp
_publ_contact_author_fax         '81 92 642 2607'
_publ_contact_author_name        'Prof. Tsutomu Katsuki'
_publ_contact_author_phone       '81 92 642 2607'
_publ_section_title
;
 Oxidation Catalysis of Nb(salan) Complexes: Asymmetric Epoxidation of
 Allylic Alcohols Using Aqueous Hydrogen Peroxide as an Oxidant
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5886
_journal_page_last               5895
_journal_paper_doi               10.1021/ja100795k
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C152 H130 Cl8 N4 Nb2 O8'
_chemical_formula_moiety         'C144 H112 N4 Nb2 O7, C4 H10 O, 4(C H2 Cl2)'
_chemical_formula_sum            'C152 H130 Cl8 N4 Nb2 O8'
_chemical_formula_weight         2610.02
_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_date             2008/02/03
_audit_creation_method
'from SHELXL97 and KenX, based on form.cif supplied from IUCr'
_audit_update_record
;
2008-02-08 Manually Edited
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2603(8)
_cell_length_b                   25.3053(11)
_cell_length_c                   25.6274(10)
_cell_measurement_reflns_used    9421
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.31
_cell_volume                     13139.0(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'KENX (Sakai, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), 
KENX, and ORTEP (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            114402
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_correction_T_min  0.9072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, G. M., 1996)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.543
_refine_diff_density_min         -1.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1597
_refine_ls_number_reflns         24010
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.5575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2384
_refine_ls_wR_factor_ref         0.2564
_reflns_number_gt                20051
_reflns_number_total             24010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100795k_si_002.cif
_cod_data_source_block           sato5E
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_database_code               4102323