Synthesis and crystal structure of topiramate azidosulfate at 90K and 298K
Priyanka, Prabhakar; Jayanna, Bidarur K.; Kiran Kumar, Haruvegowda; Vinaya; Divakara, Thayamma R.; Yathirajan, Hemmige S.; Glidewell, Christopher; Parkin, Sean; Acta Crystallographica Section E 78 (2022) 984–988; doi:10.1107/S2056989022008799

data_2244205
_publ_section_title
;
 Synthesis and crystal structure of topiramate azidosulfate at 90K and
 298K
;
_journal_coeditor_code           VM2271
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              984
_journal_page_last               988
_journal_paper_doi               10.1107/S2056989022008799
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C12 H19 N3 O8 S'
_chemical_formula_moiety         'C12 H19 N3 O8 S'
_chemical_formula_sum            'C12 H19 N3 O8 S'
_chemical_formula_weight         365.36
_chemical_name_common
;
Topiramate azidosulfate
;
_chemical_name_systematic
;
2,3:4,5-Bis-<i>O</i>-(1-methylethylidene)-\b-<i>D</i>-fructopyranose
azidosulfate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9857(4)
_cell_length_b                   9.0145(4)
_cell_length_c                   22.1621(10)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.41
_cell_volume                     1595.39(13)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.439
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
<i>SADABS</i> (Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.268
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1497 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.006(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0311P)^2^+0.3897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                3599
_reflns_number_total             3662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2271sup1.cif
_cod_data_source_block           I-90K
_cod_database_code               2244205
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.952
_shelx_hkl_checksum              24672
_shelx_res_checksum              96299