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_2007461
_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         'C20 H17 N O6'
_chemical_formula_sum            'C20 H17 N O6'
_chemical_formula_weight         367.357
_chemical_melting_point          .179E-177
_chemical_name_systematic
;cis-3,4-dihydro-2-ethoxy-4-(2-nitrophenyl)-2H,5H-pyrano[3,2-c][1]benzopyran-5-
one
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2760(10)
_cell_length_b                   15.0240(10)
_cell_length_c                   14.4480(10)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.38
_cell_measurement_theta_min      4.97
_cell_volume                     1775.9(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  0.011
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3354
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        4.02
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square tablet'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.128
_refine_ls_extinction_coef       0.0072(7)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   0.851
_refine_ls_goodness_of_fit_obs   1.026
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of independent and constrained refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.851
_refine_ls_restrained_S_obs      1.026
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0413P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.079
_refine_ls_wR_factor_obs         .071
_reflns_number_gt                1874
_reflns_number_total             3127
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1342.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0413P)^2^] 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^)+(0.0413P)^2^]
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/c'
_cod_database_code               2007461