Asymmetric Aerobic Oxidation of α-Hydroxy Acid Derivatives by C~4~-Symmetric, Vanadate-Centered, Tetrakisvanadyl(V) Clusters Derived from N-Salicylidene-α-aminocarboxylates
Chien-Tien Chen; Sampada Bettigeri; Shiue-Shien Weng; Vijay D. Pawar; Ya-Hui Lin; Cheng-Yuan Liu; Way-Zen Lee; Journal of Organic Chemistry 72 (2007) 8175–8185; doi:10.1021/jo070575f

data_4022959
_publ_section_title
;
 Asymmetric Aerobic Oxidation of \a-Hydroxy Acid Derivatives
 by C~4~-Symmetric, Vanadate-Centered, Tetrakisvanadyl(V) Clusters
 Derived from N-Salicylidene-\a-aminocarboxylates
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8175
_journal_page_last               8185
_journal_paper_doi               10.1021/jo070575f
_journal_volume                  72
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C84 H132 K N4 O25 V5'
_chemical_formula_sum            'C84 H132 K N4 O25 V5'
_chemical_formula_weight         1891.74
_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                   14.294(3)
_cell_length_b                   14.681(3)
_cell_length_c                   51.888(10)
_cell_measurement_reflns_used    139547
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     10889(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.796
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1329
_diffrn_reflns_av_sigmaI/netI    0.1488
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            46393
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         15003
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2267
_reflns_number_gt                8786
_reflns_number_total             15003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070575f-File001_3.cif
_cod_data_source_block           4562(cluster-5)
_cod_database_code               4022959