Cocrystals of zonisamide: physicochemical characterization and sustained release solid forms
Aitipamula, Srinivasulu; Cadden, Joseph; Chow, Pui Shan; CrystEngComm 20 (2018) 2923–; doi:10.1039/C8CE00084K

data_7230481
_publ_section_title
;
 Cocrystals of zonisamide: physicochemical characterization and sustained
 release solid forms
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              2923
_journal_paper_doi               10.1039/C8CE00084K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C8 H8 N2 O3 S, C6 H7 N O'
_chemical_formula_sum            'C14 H15 N3 O4 S'
_chemical_formula_weight         321.35
_chemical_name_systematic        Zonisamide-2-hydroxy-5-methylpyridine
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2018-01-12 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.2761(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1373(3)
_cell_length_b                   11.23707(18)
_cell_length_c                   9.45521(17)
_cell_measurement_reflns_used    14144
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5830
_cell_measurement_theta_min      4.2470
_cell_volume                     1441.87(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2945
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -10.00  97.00   1.00    7.25    --   18.83  57.00 -30.00  107
  2  \w     37.00 108.00   1.00    7.25    --   18.83 178.00 150.00   71
  3  \w     -4.00  97.00   1.00    7.25    --   18.83  38.00 -60.00  101
  4  \w     -8.00 103.00   1.00    7.25    --   18.83  77.00 150.00  111
  5  \w    -15.00  70.00   1.00    7.25    --   18.83  57.00  90.00   85
  6  \w    -10.00  71.00   1.00    7.25    --   18.83-111.00 179.00   81
  7  \w    -65.00  10.00   1.00    7.25    --   18.83 -38.00-150.00   75
  8  \w    -61.00  54.00   1.00    7.25    --   18.83 -57.00 -60.00  115
  9  \w    -72.00 -46.00   1.00    7.25    --  -19.61 111.00 -86.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0349881000
_diffrn_orient_matrix_UB_12      -0.0279943000
_diffrn_orient_matrix_UB_13      -0.0300386000
_diffrn_orient_matrix_UB_21      0.0373353000
_diffrn_orient_matrix_UB_22      0.0381747000
_diffrn_orient_matrix_UB_23      0.0420653000
_diffrn_orient_matrix_UB_31      0.0106752000
_diffrn_orient_matrix_UB_32      -0.0417526000
_diffrn_orient_matrix_UB_33      0.0586121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23512
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.241
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                3083
_reflns_number_total             3301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00084k2.cif
_cod_data_source_block           ZNS-HMP
_cod_depositor_comments
'Adding full bibliography for 7230481--7230482.cif.'
_cod_original_cell_volume        1441.87(4)
_cod_database_code               7230481
_chemical_oxdiff_formula         'C15 H15 N3 O4 S1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C10(H10), C4(H4), C3(H3), C2(H2), C13(H13)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_olex2_date_sample_data_collection 2017-12-14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.867