3-Phenyl-2-(piperidin-1-yl)-3,5,6,8-tetrahydro-4<i>H</i>-thiopyrano[3',4':2,3]thieno[5,4-<i>d</i>]pyrimidin-4-one
Xie, Hai; Meng, Shuang-Ming; Fan, Yue-Qin; Guo, Yong; Acta Crystallographica Section E 64 (2008) o2434–; doi:10.1107/S1600536808038683

data_2220137
_publ_section_title
3-Phenyl-2-(piperidin-1-yl)-3,5,6,8-tetrahydro-4<i>H</i>-thiopyrano[3',4':2,3]thieno[5,4-<i>d</i>]pyrimidin-4-one
_journal_coeditor_code           CV2480
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2434
_journal_paper_doi               10.1107/S1600536808038683
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C20 H21 N3 O S2'
_chemical_formula_moiety         'C20 H21 N3 O S2'
_chemical_formula_sum            'C20 H21 N3 O S2'
_chemical_formula_weight         383.52
_chemical_name_systematic
;
3-Phenyl-2-(piperidin-1-yl)-3,5,6,8-tetrahydro-4H-
thiopyrano[3',4':2,3]thieno[5,4-d]pyrimidin-4-one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.573(4)
_cell_angle_beta                 106.099(4)
_cell_angle_gamma                97.322(4)
_cell_formula_units_Z            2
_cell_length_a                   9.851(2)
_cell_length_b                   10.755(3)
_cell_length_c                   10.864(3)
_cell_measurement_reflns_used    2241
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.606
_cell_measurement_theta_min      2.239
_cell_volume                     935.0(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4908
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0458P)^2^+1.1731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                2739
_reflns_number_total             3203
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2480.cif
_cod_data_source_block           I
_cod_database_code               2220137
_cod_database_fobs_code          2220137