A tolbutamide‒metformin salt based on antidiabetic drug combinations: synthesis, crystal structure analysis and pharmaceutical properties
Jia, Lina; Wu, Songgu; Gong, Junbo; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619010647

data_2021743
_publ_section_title
;
 A tolbutamide--metformin salt based on antidiabetic drug combinations:
 synthesis, crystal structure analysis and pharmaceutical properties
;
_journal_coeditor_code           KU3246
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619010647
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C4 H12 N5 +, C12 H17 N2 O3 S -'
_chemical_formula_moiety         'C4 H12 N5 +, C12 H17 N2 O3 S -'
_chemical_formula_sum            'C16 H29 N7 O3 S'
_chemical_formula_weight         399.52
_chemical_name_systematic
;
2-[(Dimethylamino)(iminiumyl)methyl]guanidine
(butylcarbamoyl)[(4-methylbenzene)sulfonyl]azanide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.61(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9854(16)
_cell_length_b                   28.569(6)
_cell_length_c                   8.8257(18)
_cell_measurement_reflns_used    4643
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8625
_cell_measurement_theta_min      2.1386
_cell_volume                     2012.7(7)
_computing_cell_refinement       Crystalclear
_computing_data_collection       Crystalclear
_computing_data_reduction        Crystalclear
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11884
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         2.416
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       Prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+2.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                2731
_reflns_number_total             3432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ku3246sup1.cif
_cod_data_source_block           I
_cod_database_code               2021743
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              51343
_shelx_res_checksum              87564
_cod_database_fobs_code 2021743