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#$Date: 2025-08-23 02:36:08 +0300 (Sat, 23 Aug 2025) $
#$Revision: 301880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/02/8000230.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8000230
loop_
_publ_author_name
'N.N. Golovnev'
'M.S. Molokeev'
'M.K. Lesnikov'
'V.V. Atuchin'
_publ_section_title
;
 First outer-sphere 1,3-diethyl-2-thiobarbituric compounds
 [M(H2O)6](1,3-diethyl-2-thiobarbiturate)2*2H2O (M = Co2+, Ni2+): crystal
 structure, spectroscopic and thermal properties.
;
_journal_issue                   0
_journal_name_full               'Chemical Physics Letters'
_journal_page_first              54
_journal_page_last               59
_journal_paper_doi               10.1016/j.cplett.2016.04.059
_journal_volume                  653
_journal_year                    2016
_chemical_formula_moiety
;
2(C8 H11 N2 O2 S), Co H12 O6, 2(H2 O)
;
_chemical_formula_sum            'C16 H38 Co N4 O12 S2'
_chemical_formula_weight         601.55
_chemical_name_systematic
;
hexa-aqua-cobalt(II) bis(1,3-diethyl-2-thiobarbiturate) dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 114.8820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5729(13)
_cell_length_b                   18.0013(12)
_cell_length_c                   8.8812(6)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.26
_cell_volume                     2693.7(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0273
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.810
_diffrn_reflns_theta_min         2.263
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0344
_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/[σ²(Fo²)+(0.0422P)²+1.0567P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2745
_reflns_number_total             3621
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            CoH2O8DETBA2.cif
_cod_data_source_block           b
_cod_database_code               8000230
_cod_database_fobs_code          8000230
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.0000 0.08719(2) 0.2500 0.03334(10) Uani 1 2 d S T P . .
S S 0.19175(4) 0.44301(3) 0.90162(8) 0.06495(19) Uani 1 1 d . . . . .
O1 O 0.06451(9) 0.22970(8) 1.04206(17) 0.0540(4) Uani 1 1 d . . . . .
O2 O 0.17950(9) 0.19125(7) 0.66792(16) 0.0486(3) Uani 1 1 d . . . . .
N1 N 0.18680(9) 0.30397(8) 0.79206(18) 0.0396(3) Uani 1 1 d . . . . .
N3 N 0.12679(9) 0.32378(8) 0.97249(17) 0.0399(3) Uani 1 1 d . . . . .
C2 C 0.16748(11) 0.35234(10) 0.8881(2) 0.0405(4) Uani 1 1 d . . . . .
C4 C 0.10131(11) 0.24959(10) 0.9574(2) 0.0398(4) Uani 1 1 d . . . . .
C5 C 0.11830(12) 0.20473(10) 0.8508(2) 0.0448(4) Uani 1 1 d . . . . .
H5 H 0.1005 0.1558 0.8357 0.054 Uiso 1 1 calc R U . . .
C6 C 0.16078(11) 0.22977(10) 0.7656(2) 0.0383(4) Uani 1 1 d . . . . .
C7 C 0.23832(12) 0.32875(12) 0.7110(3) 0.0519(5) Uani 1 1 d . . . . .
H7A H 0.2694 0.2870 0.7025 0.062 Uiso 1 1 calc R U . . .
H7B H 0.2749 0.3664 0.7794 0.062 Uiso 1 1 calc R U . . .
C8 C 0.19069(16) 0.35996(14) 0.5409(3) 0.0688(7) Uani 1 1 d . . . . .
H8A H 0.2256 0.3729 0.4903 0.083 Uiso 1 1 calc R U . . .
H8B H 0.1629 0.4035 0.5497 0.083 Uiso 1 1 calc R U . . .
H8C H 0.1532 0.3235 0.4741 0.083 Uiso 1 1 calc R U . . .
C9 C 0.10553(15) 0.37151(12) 1.0838(3) 0.0588(6) Uani 1 1 d . . . . .
H9A H 0.1420 0.4132 1.1210 0.071 Uiso 1 1 calc R U . . .
H9B H 0.1108 0.3432 1.1807 0.071 Uiso 1 1 calc R U . . .
C10 C 0.0231(2) 0.39973(19) 0.9980(5) 0.1045(11) Uani 1 1 d . . . . .
H10A H 0.0194 0.4325 0.9097 0.125 Uiso 1 1 calc R U . . .
H10B H 0.0092 0.4263 1.0757 0.125 Uiso 1 1 calc R U . . .
H10C H -0.0126 0.3587 0.9532 0.125 Uiso 1 1 calc R U . . .
O3 O 0.00900(9) 0.09350(8) 0.02196(18) 0.0454(3) Uani 1 1 d D . . . .
H3WA H 0.0266(12) 0.1400(11) 0.021(3) 0.054 Uiso 1 1 d D U . . .
H3WB H 0.0330(13) 0.0628(12) -0.009(3) 0.054 Uiso 1 1 d D U . . .
O4 O 0.08491(8) 0.00321(7) 0.35919(19) 0.0455(3) Uani 1 1 d D . . . .
H4WA H 0.1174(12) 0.0170(13) 0.455(2) 0.055 Uiso 1 1 d D U . . .
H4WB H 0.1121(13) -0.0096(12) 0.307(3) 0.055 Uiso 1 1 d D U . . .
O5 O 0.08567(10) 0.16859(9) 0.34144(18) 0.0551(4) Uani 1 1 d D . . . .
H5WA H 0.0846(14) 0.2021(13) 0.278(3) 0.066 Uiso 1 1 d D U . . .
H5WB H 0.1134(14) 0.1838(14) 0.437(3) 0.066 Uiso 1 1 d D U . . .
O6 O 0.17027(9) 0.04161(9) 0.68084(19) 0.0516(4) Uani 1 1 d D . . . .
H6WA H 0.2113(12) 0.0234(14) 0.719(3) 0.062 Uiso 1 1 d D U . . .
H6WB H 0.1760(15) 0.0881(11) 0.683(3) 0.062 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O5 Co O5 89.41(10) 2 .
O5 Co O4 91.41(6) 2 2
O5 Co O4 175.45(6) . 2
O5 Co O4 175.45(6) 2 .
O5 Co O4 91.41(6) . .
O4 Co O4 88.12(8) 2 .
O5 Co O3 88.86(6) 2 2
O5 Co O3 86.74(6) . 2
O4 Co O3 97.74(6) 2 2
O4 Co O3 86.73(5) . 2
O5 Co O3 86.74(6) 2 .
O5 Co O3 88.86(6) . .
O4 Co O3 86.73(5) 2 .
O4 Co O3 97.74(6) . .
O3 Co O3 173.81(8) 2 .
C2 N1 C6 123.15(14) . .
C2 N1 C7 120.11(15) . .
C6 N1 C7 116.73(15) . .
C2 N3 C4 123.14(15) . .
C2 N3 C9 120.68(15) . .
C4 N3 C9 116.17(15) . .
N1 C2 N3 116.89(15) . .
N1 C2 S 121.90(13) . .
N3 C2 S 121.21(14) . .
O1 C4 C5 125.51(17) . .
O1 C4 N3 117.28(16) . .
C5 C4 N3 117.21(15) . .
C6 C5 C4 122.33(17) . .
C6 C5 H5 118.8 . .
C4 C5 H5 118.8 . .
O2 C6 C5 125.56(16) . .
O2 C6 N1 117.38(15) . .
C5 C6 N1 117.04(16) . .
N1 C7 C8 111.85(17) . .
N1 C7 H7A 109.2 . .
C8 C7 H7A 109.2 . .
N1 C7 H7B 109.2 . .
C8 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 C10 111.3(2) . .
N3 C9 H9A 109.4 . .
C10 C9 H9A 109.4 . .
N3 C9 H9B 109.4 . .
C10 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Co O3 H3WA 103.8(14) . .
Co O3 H3WB 123.8(16) . .
H3WA O3 H3WB 112(2) . .
Co O4 H4WA 109.3(16) . .
Co O4 H4WB 116.4(15) . .
H4WA O4 H4WB 107(2) . .
Co O5 H5WA 117.4(17) . .
Co O5 H5WB 132.9(17) . .
H5WA O5 H5WB 107(2) . .
H6WA O6 H6WB 109(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co O5 2.0618(14) 2
Co O5 2.0618(14) .
Co O4 2.1037(13) 2
Co O4 2.1037(13) .
Co O3 2.1042(13) 2
Co O3 2.1042(13) .
S C2 1.6841(19) .
O1 C4 1.262(2) .
O2 C6 1.268(2) .
N1 C2 1.368(2) .
N1 C6 1.406(2) .
N1 C7 1.487(2) .
N3 C2 1.369(2) .
N3 C4 1.404(2) .
N3 C9 1.483(2) .
C4 C5 1.379(3) .
C5 C6 1.378(2) .
C5 H5 0.9300 .
C7 C8 1.502(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.484(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
O3 H3WA 0.900(19) .
O3 H3WB 0.827(19) .
O4 H4WA 0.850(18) .
O4 H4WB 0.852(18) .
O5 H5WA 0.82(2) .
O5 H5WB 0.83(2) .
O6 H6WA 0.77(2) .
O6 H6WB 0.843(19) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 N1 C2 N3 5.9(3) . . . .
C7 N1 C2 N3 -173.46(16) . . . .
C6 N1 C2 S -173.64(14) . . . .
C7 N1 C2 S 7.0(2) . . . .
C4 N3 C2 N1 -3.4(3) . . . .
C9 N3 C2 N1 178.07(17) . . . .
C4 N3 C2 S 176.18(14) . . . .
C9 N3 C2 S -2.4(3) . . . .
C2 N3 C4 O1 179.76(17) . . . .
C9 N3 C4 O1 -1.6(3) . . . .
C2 N3 C4 C5 -0.5(3) . . . .
C9 N3 C4 C5 178.10(18) . . . .
O1 C4 C5 C6 -178.14(19) . . . .
N3 C4 C5 C6 2.2(3) . . . .
C4 C5 C6 O2 178.83(18) . . . .
C4 C5 C6 N1 0.1(3) . . . .
C2 N1 C6 O2 176.81(17) . . . .
C7 N1 C6 O2 -3.8(2) . . . .
C2 N1 C6 C5 -4.4(3) . . . .
C7 N1 C6 C5 174.99(17) . . . .
C2 N1 C7 C8 -90.3(2) . . . .
C6 N1 C7 C8 90.3(2) . . . .
C2 N3 C9 C10 96.7(3) . . . .
C4 N3 C9 C10 -82.0(3) . . . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168344051
