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

data_7228506
_publ_section_title
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 Ionic Cocrystals of Molecular Saccharin
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00627F
_journal_year                    2017
_chemical_formula_moiety         '0.25(C56 H44 Cs4 N8 O28 S8)'
_chemical_formula_sum            'C14 H11 Cs N2 O7 S2'
_chemical_formula_weight         516.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
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2017-01-24 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.297(2)
_cell_length_b                   6.6748(11)
_cell_length_c                   19.359(3)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      3.05
_cell_volume                     1718.2(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0731
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43638
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.858
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.385
_refine_diff_density_min         -2.333
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+27.4330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1816
_reflns_number_total             1840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00627f1.cif
_cod_data_source_block           C7H4NO3S_Cs_C7H5NO3S_H2O
_cod_database_code               7228506
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.528
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 H1A-O1
 1 with sigma of 0.02
 H1B-O1
 1 with sigma of 0.02
3. Others
 Fixed Sof: O1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N008(H1C), C00D(H00D), C00G(H00G), C00I(H00I), C00K(H00K), C00L(H00L),
 C00M(H00M), C00N(H00N), C1(H1)
;
_shelx_res_checksum              10019
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'