1,7-Dihydroxy-2,3,4-trimethoxy-9<i>H</i>-xanthen-9-one monohydrate from <i>Halenia elliptica</i>
Yu, Peizhong; Shen, Xiaojuan; Hu, Changqi; Meehan, Edward J.; Chen, Liqing; Acta Crystallographica Section E 64 (2008) o651–o652; doi:10.1107/S1600536808004832

data_2217971
_publ_section_title
;
 1,7-Dihydroxy-2,3,4-trimethoxy-9<i>H</i>-xanthen-9-one monohydrate
 from <i>Halenia elliptica</i>
;
_journal_coeditor_code           NG2424
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o651
_journal_page_last               o652
_journal_paper_doi               10.1107/S1600536808004832
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C16 H14 O7, H2 O'
_chemical_formula_moiety         'C16 H14 O7, H2 O'
_chemical_formula_sum            'C16 H16 O8'
_chemical_formula_weight         336.29
_chemical_melting_point          437
_chemical_name_common            1,7-dihydroxy-2,3,4-trimethoxyxanthone
_chemical_name_systematic
;
1,7-dihydroxy-2,3,4-trimethoxy-9H-xanthen-9-one monohydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.6830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9272(9)
_cell_length_b                   10.4511(8)
_cell_length_c                   14.0201(11)
_cell_measurement_reflns_used    3563
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.50
_cell_volume                     1487.8(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       'Thin-slice \w'
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8808
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.241
_refine_ls_extinction_coef       0.0085(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0743P)^2^+0.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                2848
_reflns_number_total             3563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2424.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217971
_cod_database_fobs_code          2217971