Noncovalent interaction network of chalcogen, halogen and hydrogen bonds for supramolecular β-sheet organization.
Cao, Jinlian; Weng, Peimin; Qi, Yuanwei; Lin, Kexin; Yan, Xiaosheng; Chemical communications (Cambridge, England) 60 (2024) 1484–1487; doi:10.1039/d3cc05539f

data_7132595
_publ_section_title
;
 Noncovalent interaction network of chalcogen, halogen and hydrogen bonds
 for supramolecular &#x3b2;-sheet organization.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1484
_journal_page_last               1487
_journal_paper_doi               10.1039/d3cc05539f
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H22 I2 N4 O4 S'
_chemical_formula_sum            'C24 H22 I2 N4 O4 S'
_chemical_formula_weight         716.31
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-30 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                84.320(5)
_cell_angle_beta                 88.126(6)
_cell_angle_gamma                87.821(6)
_cell_formula_units_Z            1
_cell_length_a                   4.7109(4)
_cell_length_b                   5.1887(3)
_cell_length_c                   25.0379(15)
_cell_measurement_reflns_used    2942
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4190
_cell_measurement_theta_min      5.3180
_cell_volume                     608.31(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -16.00   1.00    2.00    --  -41.35 -57.00   0.00   94
  2  \w    -67.00  29.00   1.00    2.00    --  -41.35  57.00 150.00   96
  3  \w     65.00 107.00   1.00    2.00    --   41.35-147.00 -25.00   42
  4  \w    -29.00  61.00   1.00    2.00    --   41.35 -37.00-150.00   90
  5  \w     83.00 123.00   1.00    8.00    --  105.38 -61.00 -30.00   40
  6  \w    121.00 162.00   1.00    8.00    --  105.38  61.00 -90.00   41
  7  \w     35.00  98.00   1.00    8.00    --  105.38 -77.00 120.00   63
  8  \w     39.00 129.00   1.00    8.00    --  105.38 -45.00-150.00   90
  9  \w     68.00 106.00   1.00    8.00    --  105.38 -94.00-150.00   38
 10  \w     43.00  71.00   1.00    8.00    --  105.38-124.00 139.00   28
 11  \w     77.00 104.00   1.00    8.00    --  105.38-124.00 139.00   27
 12  \w     47.00 128.00   1.00    8.00    --  105.38 -45.00 -60.00   81
 13  \w    110.00 169.00   1.00    8.00    --  105.38  77.00 -60.00   59
 14  \w     26.00  62.00   1.00    8.00    --  105.38 -94.00-120.00   36
 15  \w     27.00  63.00   1.00    8.00    --  105.38 -94.00-150.00   36
 16  \w     69.00 102.00   1.00    8.00    --  105.38 -94.00 -30.00   33
 17  \w     71.00 106.00   1.00    8.00    --  105.38 -94.00 -90.00   35
 18  \w     40.00 172.00   1.00    8.00    --  105.38   0.00 -90.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0128097000
_diffrn_orient_matrix_UB_12      0.0018180000
_diffrn_orient_matrix_UB_13      -0.0615448000
_diffrn_orient_matrix_UB_21      -0.3104974000
_diffrn_orient_matrix_UB_22      -0.0829621000
_diffrn_orient_matrix_UB_23      0.0011576000
_diffrn_orient_matrix_UB_31      -0.1026700000
_diffrn_orient_matrix_UB_32      0.2868517000
_diffrn_orient_matrix_UB_33      -0.0055696000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            3774
_diffrn_reflns_point_group_measured_fraction_full 0.573
_diffrn_reflns_point_group_measured_fraction_max 0.553
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.076
_diffrn_reflns_theta_min         3.549
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.445
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.128
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       plate
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.033
_refine_diff_density_max         3.137
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.001(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         2694
_refine_ls_number_restraints     301
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1330P)^2^+6.3026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.150
_reflns_Friedel_fraction_full    0.156
_reflns_Friedel_fraction_max     0.145
_reflns_number_gt                2601
_reflns_number_total             2694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05539f2.cif
_cod_data_source_block           y
_cod_depositor_comments          'Adding full bibliography for 7132595.cif.'
_cod_database_code               7132595
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H22I2N4O4S
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4.a Ternary CH refined with riding coordinates:
 C16(H16), C8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C13(H13), C5(H5), N2(H2), C2(H2A), N4(H4), N3(H3), C23(H23),
 C12(H12), N1(H1), C21(H21), C6(H6), C24(H24), C3(H3A)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              81881
_shelx_hkl_checksum              83267
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.536
_oxdiff_exptl_absorpt_empirical_full_min 0.652