Synthesis and structure of hypervalent diacetoxybromobenzene and aziridination of olefins with imino-λ3-bromane generated in situ under metal-free conditions.
Hoque, Md Mahbubul; Miyamoto, Kazunori; Tada, Norihiro; Shiro, Motoo; Ochiai, Masahito; Organic letters 13 (2011) 5428–5431; doi:10.1021/ol201868n

data_1502418
_publ_section_title
;
 Synthesis and structure of hypervalent diacetoxybromobenzene and
 aziridination of olefins with imino-\l3-bromane generated in situ under
 metal-free conditions.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5428
_journal_page_last               5431
_journal_paper_doi               10.1021/ol201868n
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C11 H10 Br F3 O4'
_chemical_formula_sum            'C11 H10 Br F3 O4'
_chemical_formula_weight         343.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 119.334(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.2071(13)
_cell_length_b                   20.451(3)
_cell_length_c                   8.7017(15)
_cell_measurement_reflns_used    10006
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.35
_cell_measurement_theta_min      4.33
_cell_volume                     1273.3(4)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2000-2010)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku, 2000-2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11102
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.876
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2245
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                1712
_reflns_number_total             2245
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol201868n_si_001.cif
_cod_data_source_block           RGK1169
_cod_original_cell_volume        1273.2(4)
_cod_database_code               1502418