Enantioselective Intramolecular Oxidative Aminocarbonylation of Alkenylureas Catalyzed by Palladium-Spiro Bis(isoxazoline) Complexes
Tetsuya Tsujihara; Toshio Shinohara; Kazuhiro Takenaka; Shinobu Takizawa; Kiyotaka Onitsuka; Minoru Hatanaka; Hiroaki Sasai; Journal of Organic Chemistry 74 (2009) 9274–9279; doi:10.1021/jo901778a

data_4025092
_publ_contact_author_address
;    The Institute of Scientific and Industrial Research
     Osaka University
     8-1 Mihogaoka, Ibaraki
     Osaka 567-0047, Japan   
;
_publ_contact_author_email       sasai@sanken.osaka-u.ac.jp
_publ_contact_author_fax         +81-6-6879-8469
_publ_contact_author_name        'Hiroaki SASAI'
_publ_contact_author_phone       +81-6-6879-8466
_publ_section_title
;
Enantioselective Intramolecular Oxidative Aminocarbonylation of
Alkenylureas Catalyzed by Palladium-Spiro Bis(isoxazoline) Complexes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9274
_journal_page_last               9279
_journal_paper_doi               10.1021/jo901778a
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C23 H38 N2 O2 '
_chemical_formula_sum            'C23 H38 N2 O2'
_chemical_formula_weight         374.57
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_audit_creation_date             2007-08-23
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.996(6)
_cell_length_b                   26.305(4)
_cell_length_c                   11.977(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    198.1
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      16.3
_cell_volume                     2204(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2002
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3214
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             824.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1764
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    3.0622    2.5938    2.0452
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                1764
_reflns_number_total             3214
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo901778a_si_003.cif
_cod_data_source_block           '_iprxa____________________'
_cod_original_formula_sum        'C23 H38 N2 O2 '
_cod_database_code               4025092