Solid Solution Polymorphs afford two High-Soluble Co-Drug Forms of Tolbutamide and Chlorpropamide
Spoletti, Enrico; Verma, Vivek; Cappuccino, Chiara; Lusi, Matteo; Chemical Communications  (2023) –; doi:10.1039/D3CC04725C

data_7132319
_publ_section_title
;
 Solid Solution Polymorphs afford two High-Soluble Co-Drug Forms of
 Tolbutamide and Chlorpropamide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04725C
_journal_year                    2023
_chemical_formula_sum            'C6.6 H7.81 Cl0.4 N O2 S'
_chemical_formula_weight         179.30
_chemical_name_common            'Toluensulfonamide Chlorobenzylsulfonamide'
_chemical_properties_physical    metastable
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2023-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                86.808(4)
_cell_angle_beta                 76.707(4)
_cell_angle_gamma                75.775(4)
_cell_formula_units_Z            8
_cell_length_a                   9.7280(14)
_cell_length_b                   9.9056(15)
_cell_length_c                   17.743(3)
_cell_measurement_reflns_used    412
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     1612.9(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31048
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.418
_diffrn_reflns_theta_min         2.428
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       needle
_exptl_crystal_F_000             745
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3639 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(18)
_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     809
_refine_ls_number_reflns         11587
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.927
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+1.2654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                8681
_reflns_number_total             11587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04725c2.cif
_cod_data_source_block           SS3_39
_cod_original_formula_sum        'C6.60 H7.81 Cl0.40 N O2 S'
_cod_database_code               7132319
_shelxl_version_number           2014-3
_shelx_res_checksum              10299
_shelx_hkl_checksum              95932