Double axial chirality promoted asymmetric [2,3] Stevens rearrangement of N-cinnamyl L-alanine amide-derived ammonium ylides
Eiji Tayama; Noriko Naganuma; Hajime Iwamoto; Eietsu Hasegawa; Chem.Commun. 50 (2014) 6860–; doi:10.1039/C4CC02536A

data_7114573
_publ_section_title
;
 Double axial chirality promoted asymmetric [2,3] Stevens rearrangement of
 N-cinnamyl L-alanine amide-derived ammonium ylides
;
_journal_name_full               Chem.Commun.
_journal_page_first              6860
_journal_paper_doi               10.1039/C4CC02536A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C32 H36 N2 O3'
_chemical_formula_sum            'C32 H36 N2 O3'
_chemical_formula_weight         496.65
_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                92.9461(12)
_cell_angle_beta                 100.8627(11)
_cell_angle_gamma                117.8884(12)
_cell_formula_units_Z            2
_cell_length_a                   11.0902(3)
_cell_length_b                   11.2800(3)
_cell_length_c                   12.2160(3)
_cell_measurement_reflns_used    8895
_cell_measurement_temperature    143
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.06
_cell_volume                     1309.25(6)
_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  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR88 (Giacovazzo, et al., 1989)'
_diffrn_ambient_temperature      143
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10978
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             532.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5557
_refine_ls_R_factor_gt           0.1041
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0400Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3840
_reflns_number_gt                4437
_reflns_number_total             5557
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc02536a2.cif
_cod_data_source_block           20140331
_cod_original_cell_volume        1309.26(6)
_cod_database_code               7114573