Structural motifs in salts of sulfathiazole: implications for design of salt forms in pharmaceuticals APIs
Seaton, Colin C.; Thomas, Rayan R.; Essifaow, Eman A. A.; Nauha, Elisa; Munshi, Tasnim; Scowen, Ian J.; CrystEngComm 20 (2018) 3428–; doi:10.1039/C8CE00606G

data_7230751
_publ_section_title
;
 Structural motifs in salts of sulfathiazole: implications for design of
 salt forms in pharmaceuticals APIs
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              3428
_journal_paper_doi               10.1039/C8CE00606G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '2(C9 H10 N3 O2 S2), 2(N O3), H N O3'
_chemical_formula_sum            'C18 H21 N9 O13 S4'
_chemical_formula_weight         699.68
_chemical_name_common            'Sulfathiazoium hydrogen dinitrate'
_chemical_name_systematic
;
4-(1,3-thiazol-2(3H)-ylidenesulfamoyl)anilinium nitrate nitric acid
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.8180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9484(4)
_cell_length_b                   8.2585(2)
_cell_length_c                   22.9621(6)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.63
_cell_volume                     2784.33(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.065
_diffrn_reflns_theta_min         1.791
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0450P)^2^+1.7483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5971
_reflns_number_total             8100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00606g2.cif
_cod_data_source_block           ee_sulfa_no3_0m
_cod_depositor_comments
'Adding full bibliography for 7230749--7230753.cif.'
_cod_original_cell_volume        2784.32(12)
_cod_database_code               7230751
_olex2_refinement_description
;
1. Others
 Sof(O1AA)=Sof(O0AA)=Sof(O2AA)=1-FVAR(1)
 Sof(O00H)=Sof(O00Q)=Sof(O00W)=FVAR(1)
 Sof(O4AA)=Sof(O3AA)=Sof(O6)=1-FVAR(2)
 Sof(O00V)=Sof(O00Y)=Sof(O018)=FVAR(2)
 Sof(O1)=Sof(O2)=Sof(O4)=1-FVAR(3)
 Sof(O6AA)=Sof(O7AA)=Sof(O5AA)=FVAR(3)
;
_shelx_res_checksum              55556
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'