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_7224522
_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 H14 N4 O2 S, C7 H5 N O3 S'
_chemical_formula_sum            'C19 H19 N5 O5 S2'
_chemical_formula_weight         461.51
_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   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                 104.488(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0729(3)
_cell_length_b                   17.6015(7)
_cell_length_c                   14.4311(6)
_cell_measurement_reflns_used    2642
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      73.3000
_cell_measurement_theta_min      4.0400
_cell_volume                     1985.38(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -41.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2343   37.0000  -90.0000 77

  2 omega  -96.00  -40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2343  125.0000  150.0000 56

  3 omega  -15.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2343   37.0000 -150.0000 51

  4 omega   18.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2343 -125.0000  120.0000 39

  5 omega   41.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2343 -125.0000   30.0000 26

  6 omega   86.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522   77.0000 -180.0000 72

  7 omega   29.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522  -30.0000 -150.0000 60

  8 omega   29.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522  -77.0000   60.0000 67

  9 omega   37.00   70.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522  -30.0000  -90.0000 33

 10 omega  113.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522  -77.0000   60.0000 26

 11 omega   39.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522  -45.0000   60.0000 52

 12 omega   72.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9522   15.0000  120.0000 101
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1863259000
_diffrn_orient_matrix_UB_12      -0.0121360000
_diffrn_orient_matrix_UB_13      0.0053141000
_diffrn_orient_matrix_UB_21      -0.0544507000
_diffrn_orient_matrix_UB_22      0.0716370000
_diffrn_orient_matrix_UB_23      -0.0613866000
_diffrn_orient_matrix_UB_31      -0.0338014000
_diffrn_orient_matrix_UB_32      -0.0488013000
_diffrn_orient_matrix_UB_33      -0.0914854000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7165
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         4.04
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0605P)^2^+0.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                2853
_reflns_number_total             3553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra27759k2.cif
_cod_data_source_block           fx141125a
_cod_original_cell_volume        1985.40(13)
_cod_database_code               7224522
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C16(H16), C2(H2), C3(H3), C4(H4), C5(H5A)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'