(4<i>R</i>)-Ethyl 4-(4-chlorophenyl)-2-hydroxy-5-oxo-2,3,4,5-tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
Wang, Yifeng; Zhang, Wei; Xu, Xiangsheng; Zhang, Guangcun; Acta Crystallographica Section E 66 (2010) o217–; doi:10.1107/S1600536809051976

data_2224825
_publ_section_title
;(4<i>R</i>)-Ethyl
 4-(4-chlorophenyl)-2-hydroxy-5-oxo-2,3,4,5-tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
;
_journal_coeditor_code           ZQ2019
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o217
_journal_paper_doi               10.1107/S1600536809051976
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C21 H17 Cl O6'
_chemical_formula_moiety         'C21 H17 Cl O6'
_chemical_formula_sum            'C21 H17 Cl O6'
_chemical_formula_weight         400.80
_chemical_name_systematic
;
(4<i>R</i>)-Ethyl 4-(4-chlorophenyl)-2-hydroxy
-5-oxo-2,3,4,5-tetrahydropyrano[3,2-<i>c</i>]chromene-2-carboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6807(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4818(3)
_cell_length_b                   14.8358(7)
_cell_length_c                   11.3403(6)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.3
_cell_volume                     919.20(8)
_computing_cell_refinement       'PROCESS-AUTO  (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO  (Rigaku, 2006)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2007)'
_computing_molecular_graphics    'Ortep3 for windows (Farrugia,1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rolling anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8978
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.198
_refine_ls_abs_structure_details 'Flack (1983), 1434 Friedel pairs'
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.080
_reflns_number_gt                3027
_reflns_number_total             3606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zq2019.cif
_cod_data_source_block           I
_cod_database_code               2224825
_cod_database_fobs_code          2224825