Total Synthesis and Structural Determination of the Dimeric Tetrahydroxanthone Ascherxanthone A.
Xiao, Zheming; Li, Yayue; Gao, Shuanhu; Organic letters 19 (2017) 1834–1837; doi:10.1021/acs.orglett.7b00592

data_1545663
_publ_section_title
;
 Total Synthesis and Structural Determination of the Dimeric
 Tetrahydroxanthone Ascherxanthone A.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1834
_journal_page_last               1837
_journal_paper_doi               10.1021/acs.orglett.7b00592
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C18 H24 O6'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.455(3)
_cell_angle_beta                 97.868(4)
_cell_angle_gamma                111.507(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7914(9)
_cell_length_b                   8.2550(9)
_cell_length_c                   16.9969(19)
_cell_measurement_reflns_used    4361
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.43
_cell_volume                     1002.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0672P)^2^+0.1227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                2772
_reflns_number_total             3528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b00592_si_004.cif
_cod_data_source_block           z
_cod_depositor_comments
'Adding full bibliography for 1545661--1545663.cif.'
_cod_original_cell_volume        1002.37(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1545663