Pharmaceutical Crystalline Complexes of Sulfamethazine with Saccharin: Same Interaction Site but Different Ionization States
Fu, Xue; Li, Jianhui; Wang, Lianyan; Wu, Bing; Xu, Xu; Deng, Zongwu; Zhang, Hailu; RSC Adv.  (2016) –; doi:10.1039/C5RA27759K

data_7224523
_publ_section_title
;
 Pharmaceutical Crystalline Complexes of Sulfamethazine with Saccharin:
 Same Interaction Site but Different Ionization States
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA27759K
_journal_year                    2016
_chemical_formula_moiety         'C12 H15 N4 O2 S, C7 H4 N O3 S'
_chemical_formula_sum            'C19 H19 N5 O5 S2'
_chemical_formula_weight         461.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-02 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5425(3)
_cell_length_b                   16.0431(4)
_cell_length_c                   25.3246(6)
_cell_measurement_reflns_used    7010
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      28.4440
_cell_measurement_theta_min      3.3290
_cell_volume                     4283.26(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   39.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6514  178.0000 -180.0000 27

  2 omega  -73.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4327  -57.0000  150.0000 38

  3 omega  -22.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4327  -57.0000  150.0000 26

  4 omega -104.00  -57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4327 -178.0000   60.0000 47

  5 omega  -23.00   19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4327  -99.0000   30.0000 42

  6 omega  -44.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4327   57.0000  -60.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0564260000
_diffrn_orient_matrix_UB_12      0.0014123000
_diffrn_orient_matrix_UB_13      -0.0152245000
_diffrn_orient_matrix_UB_21      -0.0319271000
_diffrn_orient_matrix_UB_22      -0.0199044000
_diffrn_orient_matrix_UB_23      -0.0211988000
_diffrn_orient_matrix_UB_31      -0.0180781000
_diffrn_orient_matrix_UB_32      0.0394337000
_diffrn_orient_matrix_UB_33      -0.0101642000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21676
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0398
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3426
_reflns_number_total             4376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra27759k2.cif
_cod_data_source_block           g150513a
_cod_original_cell_volume        4283.2(2)
_cod_database_code               7224523
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All H(H,H) groups
2. Restrained distances
 N4-H4A = N4-H4B
 0.8 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C5(H5), C4(H4), C9(H9), C15(H15), C16(H16), C18(H18),
 C17(H17)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_date_sample_data_collection 2015-05-13
_olex2_submission_special_instructions 'No special instructions were received'