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_2020576
_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 H6 N4, 0.5C4 H8 O2'
_chemical_formula_moiety         'C4 H6 N4, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C6 H10 N4 O'
_chemical_formula_weight         154.18
_chemical_name_systematic
;
Pyrimidine-2,4-diamine--1,4-dioxane (2/1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.243(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6282(14)
_cell_length_b                   7.2157(9)
_cell_length_c                   13.879(2)
_cell_measurement_reflns_used    5777
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      3.61
_cell_volume                     746.6(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 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 0.989
_diffrn_measured_fraction_theta_max 0.986
_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  0.0311
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4207
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.585
_diffrn_reflns_theta_min         3.930
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1388
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.3097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                1261
_reflns_number_total             1388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3636sup1.cif
_cod_data_source_block           II
_cod_database_code               2020576
_cod_database_fobs_code          2020576
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.974
_shelx_hkl_checksum              88951
_shelx_res_checksum              50169