Synthesis and Characterization of Bromonium Ylides and Their Unusual Ligand Transfer Reactions with N-Heterocycles
Masahito Ochiai; Norihiro Tada; Kentaro Murai; Satoru Goto; Motoo Shiro; Journal of the American Chemical Society 128 (2006) 9608–9609; doi:10.1021/ja063492+

data_4110796
_publ_section_title
;
 Synthesis and Characterization of Bromonium Ylides and Their Unusual
 Ligand Transfer Reactions with N-Heterocycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9608
_journal_page_last               9609
_journal_paper_doi               10.1021/ja063492+
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C9  Br F18 O4 S2, C12 H9 F3 N'
_chemical_formula_sum            'C21 H9 Br F21 N O4 S2'
_chemical_formula_weight         882.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2005-10-07
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.204(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.4499(12)
_cell_length_b                   10.4918(7)
_cell_length_c                   16.6856(12)
_cell_measurement_reflns_used    29498
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.5
_cell_volume                     2842.7(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32413
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    4.995
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.80
_refine_diff_density_min         -1.84
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5136
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1176P)^2^+9.9892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2136
_reflns_number_gt                4340
_reflns_number_total             5136
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja063492si20060519_032139.cif
_cod_data_source_block           '_RGK1225'
_cod_original_formula_sum        'C21 H9 Br F21 N O4 S2 '
_cod_database_code               4110796