Ionic Cocrystals of Molecular Saccharin
Karothu, Durga Prasad; Jahovic, Ilma; Jovanovski , Gligor; Kaitner, Branko; Naumov, Pance; CrystEngComm  (2017) –; doi:10.1039/C7CE00627F

data_7228509
_publ_section_title
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 Ionic Cocrystals of Molecular Saccharin
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00627F
_journal_year                    2017
_chemical_formula_moiety         'C14 H9 Cs2 N2 O6.5 S2'
_chemical_formula_sum            'C14 H9 Cs2 N2 O6.5 S2'
_chemical_formula_weight         639.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-08
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2017-01-24 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 93.576(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0793(14)
_cell_length_b                   9.7340(5)
_cell_length_c                   15.1308(8)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.24
_cell_volume                     3686.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27108
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.627
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.219
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1228 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.6069.
The \l/2 correction factor is 0.00150.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0470P)^2^+30.1620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             3621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00627f1.cif
_cod_data_source_block           C7H4NO3SCs_0-5H2O
_cod_original_formula_sum        'C14 H9 Cs2 N2 O6.50 S2'
_cod_database_code               7228509
_shelx_estimated_absorpt_t_max   0.486
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00J(H00J), C00L(H00L), C00N(H00N), C00O(H00O),
 C00Q(H00Q), C00R(H00R)
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_shelx_res_checksum              2489
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'