Synthesis of Oxosumanenes through Benzylic Oxidation
Toru Amaya; Maiko Hifumi; Michiaki Okada; Yasutomo Shimizu; Toshiyuki Moriuchi; Kouji Segawa; Yoichi Ando; Toshikazu Hirao; Journal of Organic Chemistry 76 (2011) 8049–8052; doi:10.1021/jo2012412

data_4026605
_publ_section_title
;
 Synthesis of Oxosumanenes through Benzylic Oxidation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8049
_journal_page_last               8052
_journal_paper_doi               10.1021/jo2012412
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C21 H10 O '
_chemical_formula_sum            'C21 H10 O'
_chemical_formula_weight         278.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.0492(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   7.68545(15)
_cell_length_b                   16.9437(3)
_cell_length_c                   9.7925(2)
_cell_measurement_reflns_used    5029
_cell_measurement_temperature    277.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.6
_cell_volume                     1242.25(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.058
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13698
_diffrn_reflns_theta_full        68.20
_diffrn_reflns_theta_max         68.20
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    0.744
_exptl_crystal_description       needle
_exptl_crystal_F_000             288.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.20
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2249
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.3493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                1633
_reflns_number_total             2249
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo2012412_si_002.cif
_cod_data_source_block           '_091110hifumi'
_cod_original_formula_sum        'C21 H10 O '
_cod_database_code               4026605