Synthesis of α-Substituted Enoximes with Nucleophiles via Nitrosoallenes.
Tanimoto, Hiroki; Yokoyama, Keiichi; Mizutani, Yusuke; Shitaoka, Takashi; Morimoto, Tsumoru; Nishiyama, Yasuhiro; Kakiuchi, Kiyomi; The Journal of organic chemistry 81 (2016) 559–574; doi:10.1021/acs.joc.5b02364

data_4031763
_publ_section_title
;
 Synthesis of \a-Substituted Enoximes with Nucleophiles via
 Nitrosoallenes.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              559
_journal_page_last               574
_journal_paper_doi               10.1021/acs.joc.5b02364
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C33 H30 Br N O4 S'
_chemical_formula_sum            'C33 H30 Br N O4 S'
_chemical_formula_weight         616.57
_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                88.9061(7)
_cell_angle_beta                 82.0333(7)
_cell_angle_gamma                79.5504(7)
_cell_formula_units_Z            2
_cell_length_a                   7.65835(18)
_cell_length_b                   7.90588(18)
_cell_length_c                   24.3938(7)
_cell_measurement_reflns_used    12030
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     1438.41(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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14402
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             636.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6556
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                5546
_reflns_number_total             6556
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo5b02364_si_005.cif
_cod_data_source_block           ky-01-028-1
_cod_depositor_comments
'Adding full bibliography for 4031763--4031767.cif.'
_cod_database_code               4031763