2-Methyl-4-oxo-6,7,8,9-tetrahydrothieno[2',3':4,5]pyrimidino[1,2-<i>a</i>]pyridine-3-carboxylic acid
Elmuradov, Burkhon Zh.; Bozorov, Khurshed A.; Okmanov, Rasul Ya.; Tashkhodjaev, Bakhodir; Shakhidoyatov, Khusnutdin M.; Acta Crystallographica Section E 67 (2011) o824–; doi:10.1107/S1600536811007902

data_2229777
_publ_section_title
;
 2-Methyl-4-oxo-6,7,8,9-tetrahydrothieno[2',3':4,5]pyrimidino[1,2-<i>a</i>]pyridine-3-carboxylic
 acid
;
_journal_coeditor_code           NK2082
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o824
_journal_paper_doi               10.1107/S1600536811007902
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C12 H12 N2 O3 S'
_chemical_formula_moiety         'C12 H12 N2 O3 S'
_chemical_formula_sum            'C12 H12 N2 O3 S'
_chemical_formula_weight         264.30
_chemical_name_systematic
;
2-Methyl-4-oxo-6,7,8,9-tetrahydrothieno[2',3':4,5]pyrimidino[1,2-
<i>a</i>]pyridine-3-carboxylic acid
;
_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'
_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                 96.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.2550(15)
_cell_length_b                   20.506(4)
_cell_length_c                   15.824(3)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     2337.0(8)
_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    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe STADI4 diffractometer'
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4297
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.54
_diffrn_standards_decay_%        4.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.504
_exptl_absorpt_correction_T_max  0.6872
_exptl_absorpt_correction_T_min  0.3463
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(Blessing, 1987)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.278
_refine_ls_extinction_coef       0.0018(3)
_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   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+2.3488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                2420
_reflns_number_total             3438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nk2082.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229777
_cod_database_fobs_code          2229777