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.
N.N. Golovnev; M.S. Molokeev; M.K. Lesnikov; V.V. Atuchin; Chemical Physics Letters 653 (2016) 54–59; doi:10.1016/j.cplett.2016.04.059

data_8000229
_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), H12 Ni O6, 2(H2 O)
;
_chemical_formula_sum            'C16 H38 N4 Ni O12 S2'
_chemical_formula_weight         601.33
_chemical_name_systematic
;
hexa-aqua-nickel(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                 114.8560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5264(10)
_cell_length_b                   17.9056(10)
_cell_length_c                   8.9010(5)
_cell_measurement_reflns_used    2800
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.27
_cell_volume                     2679.2(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 0.998
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10956
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         2.275
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6446
_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    1.491
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0395P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2202
_reflns_number_total             2773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NiH2O8DETBA2.cif
_cod_data_source_block           b
_cod_database_code               8000229
_cod_database_fobs_code          8000229
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              75134
_shelx_hkl_checksum              374