Isolation of a 1,4-diketone intermediate in oxidative dimerization of 2-hydroxyanthracene and its conversion to oxahelicene
Takashi Matsuno; Yutaro Koyama; Satoru Hiroto; Jatish Kumar; Tsuyoshi Kawai; Hiroshi Shinokubo; Chem.Commun. 51 (2015) 4607–; doi:10.1039/C5cc00764J

data_7116672
_publ_section_title
;
 Isolation of a 1,4-diketone intermediate in oxidative dimerization of
 2-hydroxyanthracene and its conversion to oxahelicene
;
_journal_name_full               Chem.Commun.
_journal_page_first              4607
_journal_paper_doi               10.1039/C5cc00764J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C72 H98 O2 Si4'
_chemical_formula_sum            'C72 H98 O2 Si4'
_chemical_formula_weight         1107.86
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-24 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                85.743(6)
_cell_angle_beta                 79.779(7)
_cell_angle_gamma                84.496(7)
_cell_formula_units_Z            2
_cell_length_a                   13.171(3)
_cell_length_b                   14.918(3)
_cell_length_c                   17.544(3)
_cell_measurement_reflns_used    8512
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.05
_cell_volume                     3371.0(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27567
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.9795
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         14803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+13.4663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2493
_refine_ls_wR_factor_ref         0.2661
_reflns_number_gt                9981
_reflns_number_total             14803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00764j2.cif
_cod_data_source_block           shelxl_1
_cod_original_cell_volume        3371.0(11)
_cod_database_code               7116672