Crystal structure, spectroscopic and thermal properties of the 1,3-diethyl-2-thiobarbiturate of Rb+, Cs+, Tl+ and NH4+ complexes
Molokeev, Maxim; Golovnev, Nikolay; Vereshchagin, Sergey; Atuchin, Victor; Polyhedron 98 (2015) 113–; doi:10.1016/j.poly.2015.05.048

data_1529240
_publ_section_title
;
 Crystal structure, spectroscopic and thermal properties of the
 1,3-diethyl-2-thiobarbiturate of Rb+, Cs+, Tl+ and NH4+ complexes
;
_journal_issue                   0
_journal_name_full               Polyhedron
_journal_page_first              113
_journal_paper_doi               10.1016/j.poly.2015.05.048
_journal_volume                  98
_journal_year                    2015
_chemical_formula_moiety         'C8 H11 N2 O2 S, H4 N'
_chemical_formula_sum            'C8 H15 N3 O2 S'
_chemical_formula_weight         217.29
_chemical_name_systematic
; 
ammonium 1,3-diethyl-2-thiobarbiturate 
;
_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           SHELXL-97
_cell_angle_alpha                98.436(4)
_cell_angle_beta                 116.059(3)
_cell_angle_gamma                109.916(4)
_cell_formula_units_Z            2
_cell_length_a                   8.472(2)
_cell_length_b                   8.853(4)
_cell_length_c                   8.964(2)
_cell_measurement_temperature    296(2)
_cell_volume                     531.8(3)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SMART APEXII'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4901
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                2112
_reflns_number_total             2598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NH4DETBA.cif
_cod_data_source_block           a
_cod_original_sg_symbol_Hall
;
-P 1
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1529240
_cod_database_fobs_code          1529240