Pseudopolymorphs of 2,6-diaminopyrimidin-4-one and 2-amino-6-methylpyrimidin-4-one: one or two tautomers present in the same crystal
Gerhardt, Valeska; Tutughamiarso, Maya; Bolte, Michael; Acta Crystallographica Section C 67 (2011) o179–o187; doi:10.1107/S0108270111013072

data_2018082
_publ_section_title
;
 Pseudopolymorphs of 2,6-diaminopyrimidin-4-one and
 2-amino-6-methylpyrimidin-4-one: one or two tautomers present in the
 same crystal
;
_journal_coeditor_code           SK3407
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o179
_journal_page_last               o187
_journal_paper_doi               10.1107/S0108270111013072
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C4 H6 N4 O , 3/2C5 H9 N O'
_chemical_formula_moiety         '2(C4 H6 N4 O), 3(C5 H9 N O)'
_chemical_formula_sum            'C23 H39 N11 O5'
_chemical_formula_weight         549.66
_chemical_name_systematic
;
2,6-diaminopyrimidin-4-one <i>N</i>-methyl-2-pyrrolidone solvate (3/2)
;
_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           SHELXL97
_cell_angle_alpha                75.558(7)
_cell_angle_beta                 78.222(8)
_cell_angle_gamma                81.363(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4550(9)
_cell_length_b                   10.0803(9)
_cell_length_c                   17.0735(15)
_cell_measurement_reflns_used    6878
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      3.41
_cell_volume                     1371.9(2)
_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 (Version 2.2; Macrae <i>et al.</i>, 2008) and XP (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 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         3.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                2940
_reflns_number_total             5116
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3407.cif
_cod_data_source_block           Ic
_cod_depositor_comments
;

2017-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C11.5 H19.5 N5.5 O2.5'
_cod_original_formula_weight         274.83
_cod_original_formula_moiety         '(C4 H6 N4 O), (C5 H9 N O)'
_cod_original_formula_units_Z            4
_cod_database_code               2018082
_cod_database_fobs_code          2018082