Novel Synthesis, Properties, and Oxidizing Ability of 11,13-Disubstituted 3,8-Methanocycloundeca[8,9-b]pyrimido [5,4-d]-furan-12(11H),14(13H)-dionylium Tetrafluoroborates
Shin-ichi Naya; Yohei Yamaguchi; Makoto Nitta; Journal of Organic Chemistry 68 (2003) 9284–9291; doi:10.1021/jo035213w

data_4022572
_publ_contact_author_email       snaya@ruri.waseda.jp
_publ_contact_author_fax         +81-3-3208-2735
_publ_contact_author_name        ' Shin-ichi Naya '
_publ_contact_author_phone       +81-3-5286-3236
_publ_section_title
;
 Novel Synthesis, Properties, and Oxidizing Ability of
 11,13-Disubstituted 3,8-Methanocycloundeca[8,9-b]pyrimido
 [5,4-d]-furan-12(11H),14(13H)-dionylium Tetrafluoroborates
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9284
_journal_page_last               9291
_journal_paper_doi               10.1021/jo035213w
_journal_volume                  68
_journal_year                    2003
_chemical_formula_moiety         'C22 H22 B F4 N3 O3 '
_chemical_formula_sum            'C22 H22 B F4 N3 O3'
_chemical_formula_weight         463.24
_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'
_audit_creation_date             2003-02-03
_audit_creation_method           'by CrystalStructure v3.10'
_cell_angle_alpha                90
_cell_angle_beta                 98.12(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.844(6)
_cell_length_b                   15.79(1)
_cell_length_c                   15.418(6)
_cell_measurement_reflns_used    10496
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_cell_volume                     2131.6(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.10'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9707
_diffrn_measured_fraction_theta_max 0.9707
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19281
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Reddish
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3217
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s^2^(Fo) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                3217
_reflns_number_total             4776
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo035213wsi20030819_022541.cif
_cod_data_source_block           '_Compd_11b_______________'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C22 H22 B F4 N3 O3 '
_cod_database_code               4022572