Hydrated pseudo-polymorphs [Na2(H2O)x](2-thiobarbiturate)2 (x = 3, 4, 5): crystal structure, spectroscopic and thermal properties
N.N. Golovnev; M.S. Molokeev; I.V. Sterkhova; V.V. Atuchin; M.Y. Sidorenko; Journal of Coordination Chemistry 69 (2016) 3219–3230; doi:10.1080/00958972.2016.1228914

data_1544282
_publ_section_title
;
 Hydrated pseudo-polymorphs [Na2(H2O)x](2-thiobarbiturate)2 (x = 3, 4, 5):
 crystal structure, spectroscopic and thermal properties
;
_journal_issue                   21
_journal_name_full               'Journal of Coordination Chemistry'
_journal_page_first              3219
_journal_page_last               3230
_journal_paper_doi               10.1080/00958972.2016.1228914
_journal_volume                  69
_journal_year                    2016
_chemical_formula_sum            'C4 H7 N2 Na O4 S'
_chemical_formula_weight         202.16
_chemical_name_systematic
;
catena-(mu~4~-2-Thiobarbiturato-O,O',S,S)-
(2-Thiobarbiturato-S)-tris(mu~2~-aqua)-aqua-di-sodium
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.7075(6)
_cell_length_b                   11.0451(10)
_cell_length_c                   20.4865(17)
_cell_measurement_reflns_used    4439
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.054
_cell_measurement_theta_min      2.712
_cell_volume                     1517.7(2)
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.1263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.054
_diffrn_reflns_theta_min         2.712
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5934
_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    1.769
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 975 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0625P)^2^+0.8355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3137
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Na2H2O4HTBA2.cif
_cod_data_source_block           b
_cod_depositor_comments
;

2023-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C8 H14 N4 Na2 O8 S2'
_cod_original_formula_weight         404.33
_cod_original_formula_units_Z            4
_cod_database_code               1544282
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              75067
_cod_database_fobs_code 1544282