14-Methoxy-2,16-dioxapentacyclo[7.7.5.0^1,21^.0^3,8^.0^10,15^]henicosa-3(8),10,12,14-tetraene-7,20-dione
Lu, Weicheng; Lian, Chaomei; Yang, Yan; Zhu, Yulin; Acta Crystallographica Section E 67 (2011) o2108–; doi:10.1107/S1600536811028972

data_2231281
_publ_section_title
;
 14-Methoxy-2,16-dioxapentacyclo[7.7.5.0^1,21^.0^3,8^.0^10,15^]henicosa-3(8),10,12,14-tetraene-7,20-dione
;
_journal_coeditor_code           RK2283
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2108
_journal_paper_doi               10.1107/S1600536811028972
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H20 O5'
_chemical_formula_moiety         'C20 H20 O5'
_chemical_formula_sum            'C20 H20 O5'
_chemical_formula_weight         340.36
_chemical_name_common
;
3,4,6,7-Tetrahydro-9-(3-methoxyphenyl)-1,8(5<i>H</i>,9<i>H</i>)-dioxo-
2<i>H</i>-[9(2)-11]-xanthene
;
_chemical_name_systematic
;
14-Methoxy-2,16-dioxapentacyclo[7.7.5.0^1,21^.0^3,8^.0^10,15^]henicosa-
3(8),10,12,14-tetraene-7,20-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.846(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0939(15)
_cell_length_b                   12.5918(17)
_cell_length_c                   12.2982(16)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.57
_cell_measurement_theta_min      2.21
_cell_volume                     1660.6(4)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2004)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2004)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>SHELXTL</i>  (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\f--and \w--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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10066
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.9695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0697P)^2^+0.3859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                2361
_reflns_number_total             3882
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            rk2283.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231281
_cod_database_fobs_code          2231281