Metal-free a-CH amination of ethers with hypervalent sulfonylimino-lamda^3^-bromane that acts as an active nitrenoid
Masahito Ochiai; Shinichi Yamane; Md. Mahbubul Hoque; Motomichi Saito; Kazunori Miyamoto; Chem.Commun.  (2012) 5280–; doi:10.1039/c2cc31523h

data_7107727
_publ_section_title
;
 Metal-free a-CH amination of ethers with hypervalent
 sulfonylimino-lamda^3^-bromane that acts as an active nitrenoid
;
_journal_name_full               Chem.Commun.
_journal_page_first              5280
_journal_paper_doi               10.1039/c2cc31523h
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C5 H8 F3 N O3 S'
_chemical_formula_sum            'C5 H8 F3 N O3 S'
_chemical_formula_weight         219.18
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      78
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.0230(9)
_cell_length_b                   8.0230(9)
_cell_length_c                   13.8300(14)
_cell_measurement_reflns_used    6074
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      3.59
_cell_volume                     890.22(17)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0420
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8777
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             448.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.250
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 938 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.12(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1996
_refine_ls_number_restraints     135
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                1362
_reflns_number_total             1996
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc31523h.txt
_cod_data_source_block           SYA-174-1
_cod_original_cell_volume        890.21(16)
_cod_database_code               7107727