A three-dimensional supramolecular network structure through hydrogen bonding and π‒π interaction: synthesis, structure, and the fluorescence detection of balsalazide disodium
Wang, Chen; You, Zi Xin; Xing, Yong-Heng; Bai, Feng-Ying; Shi, Zhan; CrystEngComm 23 (2021) 4840–4847; doi:10.1039/D1CE00373A

data_7242973
_publ_section_title
;
 A three-dimensional supramolecular network structure through hydrogen
 bonding and \p--\p interaction: synthesis, structure, and the
 fluorescence detection of balsalazide disodium
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              4840
_journal_page_last               4847
_journal_paper_doi               10.1039/D1CE00373A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C9 H3 I3 O6, C5 H4 N'
_chemical_formula_sum            'C14 H7 I3 N O6'
_chemical_formula_weight         665.91
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.7110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9598(5)
_cell_length_b                   21.9155(11)
_cell_length_c                   9.5862(5)
_cell_measurement_reflns_used    6900
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.893
_cell_measurement_theta_min      2.554
_cell_volume                     1681.46(15)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11463
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.113
_diffrn_reflns_theta_min         1.858
_exptl_absorpt_coefficient_mu    5.607
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1173 before and 0.0333 after correction.
The Ratio of minimum to maximum transmission is 0.6500.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.153
_refine_diff_density_min         -2.001
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0315P)^2^+7.5243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4332
_reflns_number_total             4822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00373a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7242972--7242974.cif.'
_cod_database_code               7242973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.231
_shelx_estimated_absorpt_t_min   0.104
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C11(H11), C10(H10)
2.b Tetrahedral OH refined with riding coordinates:
 O3(H3), O5(H5)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              57211
_shelx_hkl_checksum              53682
_olex2_submission_special_instructions 'No special instructions were received'