The cis-trans isomer transformation, spectroscopic and thermal properties of Li, Na, K 1,3-diethyl-2-thiobarbiturate complexes
Golovnev, Nikolay; Molokeev, Maxim; Vereshchagin, Sergey; Sterkhova, Irina; Atuchin, Victor; Polyhedron 85 (2015) 493–; doi:10.1016/j.poly.2014.09.011

data_1529231
_publ_section_title
;
 The cis-trans isomer transformation, spectroscopic and thermal properties
 of Li, Na, K 1,3-diethyl-2-thiobarbiturate complexes
;
_journal_issue                   0
_journal_name_full               Polyhedron
_journal_page_first              493
_journal_paper_doi               10.1016/j.poly.2014.09.011
_journal_volume                  85
_journal_year                    2015
_chemical_formula_moiety         'C8 H11 K N2 O2 S'
_chemical_formula_sum            'C8 H11 K N2 O2 S'
_chemical_formula_weight         238.35
_chemical_name_systematic
; 
Catena-(mu~6~-thiobarbiturato-O,O,O' O',S,S)potassium 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.2541(6)
_cell_length_b                   14.739(2)
_cell_length_c                   16.635(3)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.45
_cell_volume                     1043.0(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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5807
_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    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0202P)^2^+0.2451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                2265
_reflns_number_total             2743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            KDETBA.cif
_cod_data_source_block           a
_cod_original_cell_volume        1043.1(3)
_cod_original_sg_symbol_Hall
;
P 2ac 2ab
;
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               1529231
_cod_database_fobs_code          1529231