One barbiturate and two solvated thiobarbiturates containing the triply hydrogen-bonded <i>ADA</i>/<i>DAD</i> synthon, plus one ansolvate and three solvates of their coformer 2,4-diaminopyrimidine
Hützler, Wilhelm Maximilian; Egert, Ernst; Bolte, Michael; Acta Crystallographica Section C 72 (2016) –; doi:10.1107/S205322961601336X

data_2020580
_publ_section_title
;
 One barbiturate and two solvated thiobarbiturates containing the triply
 hydrogen-bonded <i>ADA</i>/<i>DAD</i> synthon, plus one ansolvate and
 three solvates of their coformer 2,4-diaminopyrimidine
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322961601336X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C4 H7 N4 +, C4 H3 N2 O2 S -, 2C3 H7 N O'
_chemical_formula_moiety         'C4 H7 N4 +, C4 H3 N2 O2 S -, 2(C3 H7 N O)'
_chemical_formula_sum            'C14 H24 N8 O4 S'
_chemical_formula_weight         400.47
_chemical_name_common
;
2,4-Diaminopyrimidinium
2-thiobarbiturate--<i>N</i>,<i>N</i>-dimethylformamide (1/2)
;
_chemical_name_systematic
;2,4-Diaminopyrimidinium
4,6-dioxo-2-sulfanylidenepyrimidin-5-ide--<i>N</i>,<i>N</i>-dimethylformamide (1/2)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.230(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0115(9)
_cell_length_b                   19.2213(14)
_cell_length_c                   12.9531(13)
_cell_measurement_reflns_used    20088
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      3.32
_cell_volume                     1994.7(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 (Version 3.8, Macrae <i>et al.</i>,  2008) and XP in
SHELXTL-Plus (Sheldrick,
2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14897
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.894
_diffrn_reflns_theta_min         3.319
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.7095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                3134
_reflns_number_total             3834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3636sup1.cif
_cod_data_source_block           VI
_cod_database_code               2020580
_cod_database_fobs_code          2020580
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.971
_shelx_hkl_checksum              45351
_shelx_res_checksum              21213