9-(4-Hydroxy-3-methoxyphenyl)-3,3,6,6-tetramethyl-3,4,5,6-tetrahydro-9<i>H</i>-xanthene-1,8(2<i>H</i>,7<i>H</i>)-dione
Hasanudin, Noorhafizah; Abdul Rahim, Aisyah Saad; Mohamed, Nornisah; Quah, Ching Kheng; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o1538–o1539; doi:10.1107/S1600536810020258

data_2226648
_publ_section_title
;
 9-(4-Hydroxy-3-methoxyphenyl)-3,3,6,6-tetramethyl-3,4,5,6-tetrahydro-9<i>H</i>-xanthene-1,8(2<i>H</i>,7<i>H</i>)-dione
;
_journal_coeditor_code           RZ2454
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1538
_journal_page_last               o1539
_journal_paper_doi               10.1107/S1600536810020258
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C24 H28 O5'
_chemical_formula_moiety         'C24 H28 O5'
_chemical_formula_sum            'C24 H28 O5'
_chemical_formula_weight         396.46
_chemical_name_systematic
;
9-(4-Hydroxy-3-methoxyphenyl)-3,3,6,6-tetramethyl-3,4,5,6-tetrahydro-
9<i>H</i>-xanthene-1,8(2<i>H</i>,7<i>H</i>)-dione
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4861(10)
_cell_length_b                   11.8659(11)
_cell_length_c                   30.087(3)
_cell_measurement_reflns_used    5544
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      2.23
_cell_volume                     4100.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker APEXII DUO CCD area-detector 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26584
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.244
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.8139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                4634
_reflns_number_total             5972
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2454.cif
_cod_data_source_block           I
_cod_original_cell_volume        4100.6(6)
_cod_database_code               2226648
_cod_database_fobs_code          2226648