Hypervalent Iodine(III)-Mediated Oxidative Decarboxylation of β,γ-Unsaturated Carboxylic Acids.
Kiyokawa, Kensuke; Yahata, Shunsuke; Kojima, Takumi; Minakata, Satoshi; Organic letters 16 (2014) 4646–; doi:10.1021/ol5022433

data_1517460
_publ_section_title
;
 Hypervalent Iodine(III)-Mediated Oxidative Decarboxylation of
 \b,\g-Unsaturated Carboxylic Acids.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4646
_journal_paper_doi               10.1021/ol5022433
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C25 H25 N O6 S2'
_chemical_formula_sum            'C25 H25 N O6 S2'
_chemical_formula_weight         499.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.1670(9)
_cell_angle_beta                 87.9430(8)
_cell_angle_gamma                74.8070(8)
_cell_formula_units_Z            2
_cell_length_a                   9.47446(17)
_cell_length_b                   10.43989(19)
_cell_length_c                   12.5041(3)
_cell_measurement_reflns_used    15572
_cell_measurement_temperature    123
_cell_measurement_theta_max      59.99
_cell_measurement_theta_min      3.54
_cell_volume                     1190.69(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19274
_diffrn_reflns_theta_full        60.02
_diffrn_reflns_theta_max         60.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     403
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.4036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                2699
_reflns_number_total             3506
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol5022433_si_002.cif
_cod_data_source_block           120
_cod_depositor_comments          'Adding full bibliography for 1517460.cif.'
_cod_database_code               1517460