9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4<i>H</i>-thieno[2',3':4,5]pyrimidino[1,2-<i>a</i>]pyridin-4-one
Bozorov, Khurshed A.; Elmuradov, Burkhon Zh.; Okmanov, Rasul Ya.; Tashkhodjaev, Bakhodir; Shakhidoyatov, Khusnutdin M.; Acta Crystallographica Section E 66 (2010) o552–o553; doi:10.1107/S1600536810004101

data_2225413
_publ_section_title
9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4<i>H</i>-thieno[2',3':4,5]pyrimidino[1,2-<i>a</i>]pyridin-4-one
_journal_coeditor_code           ZL2270
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o552
_journal_page_last               o553
_journal_paper_doi               10.1107/S1600536810004101
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C17 H16 N2 O2 S'
_chemical_formula_moiety         'C17 H16 N2 O2 S'
_chemical_formula_sum            'C17 H16 N2 O2 S'
_chemical_formula_weight         312.39
_chemical_melting_point          448(3)
_chemical_name_systematic
9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4<i>H</i>-thieno[2',3':4,5]pyrimidino[1,2-<i>a</i>]pyridin-4-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.569(3)
_cell_length_b                   11.034(2)
_cell_length_c                   8.2775(17)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1511.1(5)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1997)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1997)'
_computing_data_reduction        'X-RED  (Stoe & Cie, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer D092'
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method
; Scan width (omega) = 1.56 - 1.80, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2398
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        8.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.976
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.7486
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North <i>et al.</i>, 1968)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizmatic
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.196
_refine_ls_extinction_coef       0.0065(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.8817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                1875
_reflns_number_total             2252
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2270.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225413
_cod_database_fobs_code          2225413