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_7116670
_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            'C67.2 H91.2 N1.6 O2.4 Si3.2'
_chemical_formula_weight         1049.71
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 93.590(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            5
_cell_length_a                   13.3100(5)
_cell_length_b                   29.8304(10)
_cell_length_c                   19.4965(6)
_cell_measurement_reflns_used    19096
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.07
_cell_volume                     7725.8(5)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1586
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68957
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9401
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         15087
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0976P)^2^+6.5078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                13754
_reflns_number_total             15087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00764j2.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C67.20 H91.20 N1.60 O2.40 Si3.20'
_cod_database_code               7116670