Assemblies of salts of urea and thiourea derivatives and release of hosts from composites with calcium oxide
Brahma, Rinki; Baruah, Jubaraj Bikash; New Journal of Chemistry 47 (2023) 6211–6223; doi:10.1039/D2NJ05412D

data_7062319
_publ_section_title
;
 Assemblies of salts of urea and thiourea derivatives and release of hosts
 from composites with calcium oxide
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6211
_journal_page_last               6223
_journal_paper_doi               10.1039/D2NJ05412D
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C13 H13 N3 S'
_chemical_formula_sum            'C13 H13 N3 S'
_chemical_formula_weight         243.334
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-22 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.216(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9160(4)
_cell_length_b                   22.1005(16)
_cell_length_c                   9.9693(5)
_cell_measurement_reflns_used    1396
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.7700
_cell_measurement_theta_min      2.7900
_cell_volume                     1282.79(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2760
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_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     63.00  95.00   1.00   15.99    --   20.92 178.00   0.00   32
  2  \w     17.00  78.00   1.00   15.99    --   20.92  19.00  30.00   61
  3  \w    -31.00  94.00   1.00   15.99    --   20.92   0.00 150.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0372042000
_diffrn_orient_matrix_UB_12      -0.0055842000
_diffrn_orient_matrix_UB_13      -0.0626887000
_diffrn_orient_matrix_UB_21      -0.0530986000
_diffrn_orient_matrix_UB_22      0.0272143000
_diffrn_orient_matrix_UB_23      -0.0269191000
_diffrn_orient_matrix_UB_31      0.1031623000
_diffrn_orient_matrix_UB_32      0.0160808000
_diffrn_orient_matrix_UB_33      0.0238137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5590
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9991
_diffrn_reflns_theta_full        25.0400
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             512.756
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.2109
_refine_diff_density_min         -0.2403
_refine_diff_density_rms         0.0529
_refine_ls_d_res_high            0.8396
_refine_ls_d_res_low             7.3367
_refine_ls_goodness_of_fit_ref   1.0614
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0614
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.2268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -7
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1630
_reflns_number_total             2256
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05412d3.cif
_cod_data_source_block           Phenthiourea
_cod_depositor_comments
'Adding full bibliography for 7062311--7062319.cif.'
_cod_database_code               7062319
_diffrn_oxdiff_ac4_digest_frames
;
018f431063bf0bd2cf55f4b2de3b1d431600027e87d
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2a), C1(H1a), C6(H6), C5(H5), C13(H13), C12(H12), C11(H11),
 C10(H10)
;
_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 2.788
_oxdiff_exptl_absorpt_empirical_full_min 0.612