3-[(1<i>Z</i>)-1-Hydroxy-3-oxobut-1-en-1-yl]-7-methyl-2<i>H</i>,5<i>H</i>-pyrano[4,3-<i>b</i>]pyran-2,5-dione
N. Bouhaine; A. Gherrou; A. van der Lee; Acta Crystallographica Section E 62 (2006) o5401–o5403; doi:10.1107/S1600536806045065

data_2211327
_publ_section_title
3-[(1<i>Z</i>)-1-Hydroxy-3-oxobut-1-en-1-yl]-7-methyl-2<i>H</i>,5<i>H</i>-pyrano[4,3-<i>b</i>]pyran-2,5-dione
_journal_coeditor_code           CI2201
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5401
_journal_page_last               o5403
_journal_paper_doi               10.1107/S1600536806045065
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C13 H10 O6'
_chemical_formula_moiety         'C13 H10 O6'
_chemical_formula_sum            'C13 H10 O6'
_chemical_formula_weight         262.22
_chemical_name_systematic
;
3-[(1Z)-1-Hydroxy-3-oxobut-1-en-1-yl]-7-methyl-2H,5H-pyrano[4,3-b]pyran-
2,5-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
_cell_angle_alpha                90
_cell_angle_beta                 133.882(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8290(4)
_cell_length_b                   14.1820(5)
_cell_length_c                   12.5238(5)
_cell_measurement_reflns_used    1339
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.345
_cell_measurement_theta_min      2.679
_cell_volume                     1130.27(9)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker--Nonius, 2004)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>,  2003)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX 2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26469
_diffrn_reflns_theta_full        33.177
_diffrn_reflns_theta_max         33.177
_diffrn_reflns_theta_min         2.675
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '30 frames'
_diffrn_standards_number         '2 frames'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0217
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000399
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
  w = [1-(F~o~-F~c~)^2^/36\s^2^(F)]^2^/[10.2T~0~(x)+13.2T~1~(x)+3.67T~2~(x)]
 where T~i~ are Chebychev polynomials and x = F~c~/F~max~
 (Prince, 1982; Watkin, 1994)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0856
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                2755
_reflns_number_total             4322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2201.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211327
_cod_database_fobs_code          2211327