Mechanosynthesis of pharmaceutically relevant sulfonyl-(thio)ureas
Davin Tan; Vjekoslav Strukil; Cristina Mottillo; Tomislav Friscic; Chem.Commun. 50 (2014) 5248–; doi:10.1039/C3CC47905F

data_7112631
_publ_section_title
;
 Mechanosynthesis of pharmaceutically relevant sulfonyl-(thio)ureas
;
_journal_name_full               Chem.Commun.
_journal_page_first              5248
_journal_paper_doi               10.1039/C3CC47905F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(C14 H12 N3 O4 S2), 2.5(C3 H6 O1), K2'
_chemical_formula_sum            'C35.5 H39 K2 N6 O10.5 S4'
_chemical_formula_weight         924.17
_chemical_name_common
'Potassium (4-nitrophenylcarbamothioyl)(tosyl)amide'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.650(2)
_cell_angle_beta                 93.736(2)
_cell_angle_gamma                96.762(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3664(12)
_cell_length_b                   16.466(3)
_cell_length_c                   18.699(3)
_cell_measurement_reflns_used    2340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.30
_cell_volume                     2134.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21256
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+0.0107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                3987
_reflns_number_total             7955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47905f.txt
_cod_data_source_block           cm44_0m
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35.50 H39 K2 N6 O10.50 S4'
_cod_database_code               7112631