Enantioselective Prevost and Woodward reactions using chiral hypervalent iodine(III): switchover of stereochemical course of an optically active 1,3-dioxolan-2-yl cation
Morifumi Fujita; Mikimasa Wakita; Takashi Sugimura; Chem.Commun. 47 (2011) 3983–; doi:10.1039/c1cc10129c

data_7106159
_publ_section_title
;
 Enantioselective Prevost and Woodward reactions using chiral hypervalent
 iodine(III): switchover of stereochemical course of an optically active
 1,3-dioxolan-2-yl cation
;
_journal_name_full               Chem.Commun.
_journal_page_first              3983
_journal_paper_doi               10.1039/c1cc10129c
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C22 H31 I O10, 0.5(H2 O)'
_chemical_formula_sum            'C22 H32 I O10.5'
_chemical_formula_weight         591.39
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      170
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   23.3688(11)
_cell_length_b                   23.3688(11)
_cell_length_c                   8.5888(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0
_cell_volume                     4062.0(3)
_computing_cell_refinement       'Rigaku Diffractometer Controller'
_computing_data_collection       'Rigaku Diffractometer Controller'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293.1
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Quantum CCD1 on Rigaku AFC-7R'
_diffrn_measurement_method       PHIOMEGA
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            36435
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.2109
_exptl_absorpt_correction_T_min  0.4273
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
HIGASHI, T. (1995). Abscor - Empirical Absorption Correction,
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1806.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.45
_refine_diff_density_min         -0.75
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2838 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_coef       825(55)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5061
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                5047
_reflns_number_total             6141
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c1cc10129c.txt
_cod_data_source_block           '_5-yy-04'
_cod_original_formula_sum        'C22 H32 I O10.50 '
_cod_database_code               7106159