Diethyl 2-{[(5-oxo-5<i>H</i>-thiochromeno[2,3-<i>b</i>]pyridin-7-yl)amino]methylidene}propanedioate
Khan, Muhammad Naeem; Tahir, M. Nawaz; Khan, Misbahul Ain; Munawar, Munawar Ali; Ather, Abdul Qayyum; Acta Crystallographica Section E 67 (2011) o1348–; doi:10.1107/S1600536811016291

data_2230284
_publ_section_title
;
 Diethyl
 2-{[(5-oxo-5<i>H</i>-thiochromeno[2,3-<i>b</i>]pyridin-7-yl)amino]methylidene}propanedioate
;
_journal_coeditor_code           DN2678
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1348
_journal_paper_doi               10.1107/S1600536811016291
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H18 N2 O5 S'
_chemical_formula_moiety         'C20 H18 N2 O5 S'
_chemical_formula_sum            'C20 H18 N2 O5 S'
_chemical_formula_weight         398.42
_chemical_name_systematic
;
Diethyl 2-{[(5-oxo-5<i>H</i>-thiochromeno[2,3-<i>b</i>]pyridin-7-
yl)amino]methylidene}propanedioate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 94.330(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8013(7)
_cell_length_b                   7.5180(3)
_cell_length_c                   36.2743(15)
_cell_measurement_reflns_used    1789
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.25
_cell_volume                     3753.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
PLATON (Spek, 2009)'
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       \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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3314
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                1776
_reflns_number_total             3314
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2678.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230284
_cod_database_fobs_code          2230284