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_2020581
_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 -, 2(C4 H9 N O)'
_chemical_formula_moiety         'C4 H7 N4 +, C4 H3 N2 O2 S -, 2(C4 H9 N O)'
_chemical_formula_sum            'C16 H28 N8 O4 S'
_chemical_formula_weight         428.52
_chemical_name_common
;
2,4-Diaminopyrimidinium 2-thiobarbiturate--<i>N</i>,<i>N</i>-dimethylacetamide
(1/2)
;
_chemical_name_systematic
'2,4-Diaminopyrimidinium 4,6-dioxo-2-sulfanylidene--<i>N</i>,<i>N</i>-dimethylacetamide (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                 88.151(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8868(12)
_cell_length_b                   17.2380(14)
_cell_length_c                   12.8571(14)
_cell_measurement_reflns_used    12893
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      3.36
_cell_volume                     2190.1(4)
_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
;
SHELXL2014 (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 0.988
_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  0.0592
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.889
_diffrn_reflns_theta_min         3.484
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4205
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                2955
_reflns_number_total             4205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3636sup1.cif
_cod_data_source_block           VII
_cod_database_code               2020581
_cod_database_fobs_code          2020581
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              94027
_shelx_res_checksum              92977