Base-mediated three-component system for the synthesis of <i>S</i>-substituted <i>N</i>-acyl ureas.
Shandu, Malibongwe P.; Ngwenya, Andile R.; Lamola, Jairus L.; Moshapo, Paseka T.; RSC advances 15 (2025) 44246–44251; doi:10.1039/d5ra05563f

data_7251376
_publ_section_title
;
 Base-mediated three-component system for the synthesis of
 <i>S</i>-substituted <i>N</i>-acyl ureas.
;
_journal_issue                   52
_journal_name_full               'RSC advances'
_journal_page_first              44246
_journal_page_last               44251
_journal_paper_doi               10.1039/d5ra05563f
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C11 H14 N2 O2 S'
_chemical_formula_sum            'C11 H14 N2 O2 S'
_chemical_formula_weight         238.30
_chemical_name_systematic        S-benzyl-(N,N-dimethyl-carbonyl)carbamothioate
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2025-05-16 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.544(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.8421(3)
_cell_length_b                   9.9787(5)
_cell_length_c                   10.4247(5)
_cell_measurement_reflns_used    6242
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.7322
_cell_measurement_theta_min      2.8538
_cell_volume                     595.43(5)
_computing_cell_refinement       'SAINT 8.40B (Bruker-AXS, 2022)'
_computing_data_collection       'APEX4 v2022.1.1 (Bruker-AXS, 2023)'
_computing_data_reduction        'SAINT 8.40B (Bruker-AXS, 2022)'
_computing_molecular_graphics    (Olex2)
_computing_publication_material  encifer
_computing_structure_refinement  'SHELXL-2019 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Fixed-Chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Photon3 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Incoatec I\mS multilayer optics'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10468
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.270
_diffrn_reflns_theta_min         1.994
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             252
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform and n-hexane'
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0575P)^2^+0.2015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2471
_reflns_number_total             2678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05563f2.cif
_cod_data_source_block           25pm_L_173K
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7251376
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              12777