5-Hydroxy-8,8-dimethyl-10-(2-methylbut-3-en-2-yl)-2<i>H</i>,6<i>H</i>-7,8-dihydropyrano[3,2-<i>g</i>]chromene-2,6-dione
Fun, Hoong-Kun; Sripisut, Tawanun; Laphookhieo, Surat; Chantrapromma, Suchada; Acta Crystallographica Section E 67 (2011) o422–o423; doi:10.1107/S1600536811001565

data_2228954
_publ_section_title
;
 5-Hydroxy-8,8-dimethyl-10-(2-methylbut-3-en-2-yl)-2<i>H</i>,6<i>H</i>-7,8-dihydropyrano[3,2-<i>g</i>]chromene-2,6-dione
;
_journal_coeditor_code           BQ2271
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o422
_journal_page_last               o423
_journal_paper_doi               10.1107/S1600536811001565
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C19 H20 O5'
_chemical_formula_moiety         'C19 H20 O5'
_chemical_formula_sum            'C19 H20 O5'
_chemical_formula_weight         328.35
_chemical_melting_point_gt       410
_chemical_melting_point_lt       411
_chemical_name_systematic
5-Hydroxy-8,8-dimethyl-10-(2-methylbut-3-en-2-yl)-2<i>H</i>,6<i>H</i>-7,8-dihydropyrano[3,2-<i>g</i>]chromene-2,6-dione
_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                 93.1080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2239(2)
_cell_length_b                   11.3090(3)
_cell_length_c                   13.8764(3)
_cell_measurement_reflns_used    3114
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.97
_cell_measurement_theta_min      5.84
_cell_volume                     1602.06(6)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0095
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48432
_diffrn_reflns_theta_full        71.97
_diffrn_reflns_theta_max         71.97
_diffrn_reflns_theta_min         5.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.7744
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.837
_refine_ls_extinction_coef       0.041(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.4129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                3088
_reflns_number_total             3114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bq2271.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228954
_cod_database_fobs_code          2228954