4-Hydroxy-3-[(4-hydroxy-6-methyl-2-oxo-3,6-dihydro-2<i>H</i>-pyran-3-yl)(3-thienyl)methyl]-6-methyl-3,6-dihydro-2<i>H</i>-pyran-2-one
Asad, Mohammad; Oo, Chuan-Wei; Osman, Hasnah; Hemamalini, Madhukar; Fun, Hoong-Kun; Acta Crystallographica Section E 67 (2011) o494–o495; doi:10.1107/S1600536811002716

data_2229208
_publ_section_title
;
 4-Hydroxy-3-[(4-hydroxy-6-methyl-2-oxo-3,6-dihydro-2<i>H</i>-pyran-3-yl)(3-thienyl)methyl]-6-methyl-3,6-dihydro-2<i>H</i>-pyran-2-one
;
_journal_coeditor_code           RZ2545
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o494
_journal_page_last               o495
_journal_paper_doi               10.1107/S1600536811002716
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C17 H14 O6 S'
_chemical_formula_moiety         'C17 H14 O6 S'
_chemical_formula_sum            'C17 H14 O6 S'
_chemical_formula_weight         346.34
_chemical_name_systematic
;
4-Hydroxy-3-[(4-hydroxy-6-methyl-2-oxo-3,6-dihydro-2<i>H</i>-pyran-3-yl)(3-
thienyl)methyl]-6-methyl-3,6-dihydro-2<i>H</i>-pyran-2-one
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            16
_cell_length_a                   30.6120(18)
_cell_length_b                   7.9982(5)
_cell_length_c                   25.6540(15)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.55
_cell_volume                     6281.1(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      100.00(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker APEXII DUO CCD area-detector
;
_diffrn_measurement_method       '\f and \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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            127650
_diffrn_reflns_theta_full        30.69
_diffrn_reflns_theta_max         30.69
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.9016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.753
_refine_ls_abs_structure_details 'Flack (1983), 9485 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         19406
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          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^)+(0.0845P)^2^+2.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                18459
_reflns_number_total             19406
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2545.cif
_cod_data_source_block           I
_cod_database_code               2229208
_cod_database_fobs_code          2229208