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_7116671
_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_sum            'C72 H96 O Si4'
_chemical_formula_weight         1089.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_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                90.00
_cell_angle_beta                 111.807(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.768(3)
_cell_length_b                   21.986(4)
_cell_length_c                   16.670(3)
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.21
_cell_volume                     6727(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37608
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9504
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+13.8463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2738
_reflns_number_gt                6978
_reflns_number_total             11830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00764j2.cif
_cod_data_source_block           13107yk
_cod_original_cell_volume        6726(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7116671