Five 3,4-Dihydro-2<i>H</i>,5<i>H</i>-pyrano[3,2-<i>c</i>][1]benzopyran-5-one Derivatives
Casalone, Gianluigi; Pilati, Tullio; Binello, Arianna; Acta Crystallographica Section C 54 (1998) 1042–1047; doi:10.1107/S0108270198000249

data_2007462
_publ_section_title
;
 Five
 3,4-Dihydro-2<i>H</i>,5<i>H</i>-pyrano[3,2-<i>c</i>][1]benzopyran-5-one
 Derivatives
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1042
_journal_page_last               1047
_journal_paper_doi               10.1107/S0108270198000249
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C22 H20 O6'
_chemical_formula_sum            'C22 H20 O6'
_chemical_formula_weight         380.38
_chemical_melting_point          145
_chemical_name_systematic
;3,4-dihydro-2-ethoxy-4-methoxycarbonyl-4-phenyl-2H,5H-pyrano[3,2-c][1]benzo
 pyran-5-one
;
_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                90.00
_cell_angle_beta                 107.394(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3920(10)
_cell_length_b                   17.1920(10)
_cell_length_c                   11.1930(10)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.27
_cell_measurement_theta_min      3.40
_cell_volume                     1908.3(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
'SHELXL93. Other programs used include PARSTCIF (Nardelli, 1991)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q/\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  0.030
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5977
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        3.75
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.140
_refine_ls_extinction_coef       0.0063(10)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of independent and constrained refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         2993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.072
_refine_ls_R_factor_gt           0.040
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0483P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.100
_refine_ls_wR_factor_obs         .088
_reflns_number_gt                2011
_reflns_number_total             2993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1342.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0483P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0483P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007462