Two polymorphs and the diethylammonium salt of the barbiturate eldoral
Gelbrich, Thomas; Rossi, Denise; Griesser, Ulrich J.; Acta Crystallographica Section C 68 (2012) o65–o70; doi:10.1107/S0108270111055120

data_2018393
_publ_section_title
;
 Two polymorphs and the diethylammonium salt of the barbiturate eldoral
;
_journal_coeditor_code           SK3420
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o65
_journal_page_last               o70
_journal_paper_doi               10.1107/S0108270111055120
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C4 H12 N + , C11 H16 N3 O3 -'
_chemical_formula_moiety         'C4 H12 N +, C11 H16 N3 O3 -'
_chemical_formula_sum            'C15 H28 N4 O3'
_chemical_formula_weight         312.41
_chemical_name_systematic
;
diethylammonium 5-ethyl-2,4,6-trioxo-5-(piperidin-1-yl)-1,3-diazinan-1-ide
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.8270(3)
_cell_length_b                   16.1719(4)
_cell_length_c                   18.6774(5)
_cell_measurement_reflns_used    13761
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.2496
_cell_measurement_theta_min      3.6123
_cell_volume                     3572.33(16)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2003)'
_computing_molecular_graphics
;
XP in SHELXTL (Bruker, 1998) and Mercury (Macrae <i>et al.</i>,
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_detector_area_resol_mean 10.3575
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby Gemini Ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25972
_diffrn_reflns_theta_full        67.36
_diffrn_reflns_theta_max         67.36
_diffrn_reflns_theta_min         5.20
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.212
_refine_ls_extinction_coef       0.00061(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0561P)^2^+0.9238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                2921
_reflns_number_total             3209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3420.cif
_cod_data_source_block           II
_cod_original_cell_volume        3572.35(16)
_cod_database_code               2018393
_cod_database_fobs_code          2018393