Five pseudopolymorphs of 6-amino-2-thiouracil: absence of N—H···S hydrogen bonds
Hützler, Wilhelm Maximilian; Bolte, Michael; Acta Crystallographica Section C 69 (2013) 93–100; doi:10.1107/S010827011204930X

data_2018748
_publ_section_title
;
 Five pseudopolymorphs of 6-amino-2-thiouracil: absence of
 N---H&#x00B7;&#x00B7;&#x00B7;S hydrogen bonds
;
_journal_coeditor_code           FG3285
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              93
_journal_page_last               100
_journal_paper_doi               10.1107/S010827011204930X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2C4 H5 N3 O S, 3C5 H9 N O'
_chemical_formula_moiety         '2(C4 H5 N3 O S), 3(C5 H9 N O)'
_chemical_formula_sum            'C23 H37 N9 O5 S2'
_chemical_formula_weight         583.74
_chemical_name_systematic
;
6-Amino-2-thiouracil 1-methylpyrrolidin-2-one sesquisolvate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2293(10)
_cell_length_b                   7.5483(4)
_cell_length_c                   25.1871(13)
_cell_measurement_reflns_used    28863
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.43
_cell_volume                     2895.4(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008) and XP in SHELXTL-Plus (Sheldrick,
2008)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Genix 3D multilayer optics'
_diffrn_radiation_source         'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8280
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.9248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(X-AREA; Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.338
_refine_ls_abs_structure_details 'Flack (1983), 1810 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         4332
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0660P)^2^+4.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1698
_reflns_number_gt                3541
_reflns_number_total             4332
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3285.cif
_cod_data_source_block           Id
_cod_database_code               2018748
_cod_database_fobs_code          2018748