Ethyl 2-hydroxy-5-oxo-4-phenyl-2,3,4,5-tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
Zhang, Wei; Zhang, Guangcun; Li, Bailin; Wang, Yifeng; Acta Crystallographica Section E 65 (2009) o1969–; doi:10.1107/S1600536809028311

data_2222834
_publ_section_title
;Ethyl
 2-hydroxy-5-oxo-4-phenyl-2,3,4,5-tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
;
_journal_coeditor_code           PK2181
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1969
_journal_paper_doi               10.1107/S1600536809028311
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C21 H18 O6'
_chemical_formula_moiety         'C21 H18 O6'
_chemical_formula_sum            'C21 H18 O6'
_chemical_formula_weight         366.37
_chemical_name_systematic
;
Ethyl 2-hydroxy-5-oxo-4-phenyl-2,3,4,5-
tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.5487(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   5.4988(2)
_cell_length_b                   14.9975(5)
_cell_length_c                   21.3420(10)
_cell_measurement_reflns_used    11365
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     1740.48(12)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CrystalStructure (Rigaku, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16523
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.44
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             768.00
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.19
_refine_ls_extinction_coef       0.0057(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.013P)^2^+P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                2568
_reflns_number_total             3422
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            pk2181.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2222834
_cod_database_fobs_code          2222834