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_4025093
_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         'C46 H76 B2 F8 N4 O4 Pd '
_chemical_formula_sum            'C46 H76 B2 F8 N4 O4 Pd'
_chemical_formula_weight         1029.14
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2007-08-24
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.74(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   21.325(9)
_cell_length_b                   15.977(4)
_cell_length_c                   61.30(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    143.1
_cell_measurement_theta_max      8.9
_cell_measurement_theta_min      7.9
_cell_volume                     20742(14)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.104
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            15551
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        -7.57
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8640.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.98
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         6137
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.0176
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    2.6997    1.7659    1.9622
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                6133
_reflns_number_total             13540
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo901778a_si_004.cif
_cod_data_source_block           '_rac-iPr-SPRIX-PdBF4'
_cod_original_formula_sum        'C46 H76 B2 F8 N4 O4 Pd '
_cod_database_code               4025093