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_2018749
_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           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   7.5509(7)
_cell_length_b                   15.2328(12)
_cell_length_c                   50.601(3)
_cell_measurement_reflns_used    6864
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      1.40
_cell_volume                     5820.2(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.1569
_diffrn_reflns_av_sigmaI/netI    0.1303
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            30686
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.9771
_exptl_absorpt_correction_T_min  0.9357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(X-AREA; Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1082P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2288
_reflns_number_gt                2211
_reflns_number_total             5484
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3285.cif
_cod_data_source_block           Ie
_cod_database_code               2018749
_cod_database_fobs_code          2018749