Supramolecular Assemblies of Melamine-2-Thiobarbiturate and Melamine-Barbiturate-2-Thiobarbiturate: Experimental and Theoretical Studies
Moskalenko, Ivan V.; Shilovskikh, Vladimir V.; Nesterov, Pavel V.; Novikov, Alexander S.; Omarova, Malika; Sadovnichii, Roman V.; Gurzhiy, Vladislav V.; Orekhov, Nikita D.; Skorb, Ekaterina V.; Crystals 13 (2023) 1302–; doi:10.3390/cryst13091302

data_1569817
_publ_section_title
;
 Supramolecular Assemblies of Melamine-2-Thiobarbiturate and
 Melamine-Barbiturate-2-Thiobarbiturate: Experimental and Theoretical
 Studies
;
_journal_issue                   9
_journal_name_full               Crystals
_journal_page_first              1302
_journal_paper_doi               10.3390/cryst13091302
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C4 H3 N2 O2 S, 2(H2 O), C3 H7 N6'
_chemical_formula_sum            'C7 H14 N8 O4 S'
_chemical_formula_weight         306.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-07-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.698(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7987(3)
_cell_length_b                   17.7255(4)
_cell_length_c                   6.76698(19)
_cell_measurement_reflns_used    3440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2820
_cell_measurement_theta_min      4.1010
_cell_volume                     1295.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -21.00  12.00   0.50    1.60    --  -47.38  17.00-132.00   66
  2  \w   -172.00-137.00   0.50    6.00    -- -105.93 -17.00  58.00   70
  3  \w     37.00  98.00   0.50    6.00    --  105.93-110.00-103.00  122
  4  \w     36.00 113.00   0.50    6.00    --  105.93-145.00-171.00  154
  5  \w    -93.00 -64.00   0.50    1.60    --  -47.38 125.00  73.00   58
  6  \w    -45.00 -17.00   0.50    1.60    --  -47.38 125.00  73.00   56
  7  \w   -113.00 -85.00   0.50    1.60    --  -47.38-125.00 120.00   56
  8  \w    -23.00  25.00   0.50    1.60    --  -47.38  19.00   0.00   96
  9  \w     -8.00  22.00   0.50    1.60    --   47.38 -19.00 -30.00   60
 10  \w    -67.00 -34.00   0.50    6.00    -- -105.93  61.00 -60.00   66
 11  \w    -69.00 -33.00   0.50    6.00    -- -105.93  61.00  90.00   72
 12  \w   -130.00 -97.00   0.50    6.00    -- -105.93 -17.00  58.00   66
 13  \w     64.00 103.00   0.50    6.00    --  105.93 -94.00 -90.00   78
 14  \w   -108.00 -57.00   0.50    6.00    -- -105.93 125.00  73.00  102
 15  \w   -103.00 -74.00   0.50    1.60    --  -47.38-125.00  60.00   58
 16  \w     92.00 118.00   0.50    1.60    --   47.38 125.00  73.00   52
 17  \w   -127.00 -98.00   0.50    6.00    -- -105.93 -15.00   0.00   58
 18  \w   -176.00-132.00   0.50    6.00    -- -105.93 -15.00   0.00   88
 19  \w     71.00 100.00   0.50    6.00    --  105.93 -94.00 -30.00   58
 20  \w     43.00  69.00   0.50    6.00    --  105.93 -61.00 -60.00   52
 21  \w     33.00  65.00   0.50    6.00    --  105.93 -61.00 -30.00   64
 22  \w     33.00  58.00   0.50    6.00    --  105.93 -61.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0761196000
_diffrn_orient_matrix_UB_12      0.0154183000
_diffrn_orient_matrix_UB_13      -0.1868159000
_diffrn_orient_matrix_UB_21      -0.1167657000
_diffrn_orient_matrix_UB_22      -0.0121107000
_diffrn_orient_matrix_UB_23      -0.1291670000
_diffrn_orient_matrix_UB_31      -0.0307667000
_diffrn_orient_matrix_UB_32      0.0846375000
_diffrn_orient_matrix_UB_33      0.0155454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6364
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.986
_diffrn_reflns_theta_min         4.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent colorless'
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       lamina
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0607P)^2^+0.2228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1940
_reflns_number_total             2288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ThioBarb_mel_1_last.cif
_cod_data_source_block           thiobarb_mel_1
_cod_database_code               1569817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N8(H8), N11(H11), C18(H18)
2.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N7(H7A,H7B), N10(H10A,H10B)
;
_shelx_res_checksum              85745
_shelx_hkl_checksum              73979
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.650