Zwitterionic iodonium species afford halogen bond-based porous organic frameworks
Soldatova, Natalia S.; Postnikov, Pavel S.; Ivanov, Daniil M.; Semyonov, Oleg V.; Kukurina, Olga S.; Guselnikova, Olga; Yamauchi, Yusuke; Wirth, Thomas; Zhdankin, Viktor V.; Yusubov, Mekhman S.; Gomila, Rosa M.; Frontera, Antonio; Resnati, Giuseppe; Kukushkin, Vadim Yu.; Chemical Science  (2022) –; doi:10.1039/D2SC00892K

data_1566876
_publ_section_title
;
 Zwitterionic iodonium species afford halogen bond-based porous organic
 frameworks
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00892K
_journal_year                    2022
_chemical_formula_moiety         'C15 H15 I O3 S'
_chemical_formula_sum            'C15 H15 I O3 S'
_chemical_formula_weight         402.23
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-13 deposited with the CCDC.	2022-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   20.7704(4)
_cell_length_b                   20.7704(4)
_cell_length_c                   21.5736(4)
_cell_measurement_reflns_used    8896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8600
_cell_measurement_theta_min      4.2310
_cell_volume                     8060.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     49.00  92.00   1.00    4.20    --   40.13  77.00   0.00   43
  2  \w    100.00 155.00   1.00   17.00    --  113.00  77.00  30.00   55
  3  \w    133.00 159.00   1.00   17.00    --  113.00  77.00 -60.00   26
  4  \w     79.00 146.00   1.00   17.00    --  113.00  77.00  60.00   67
  5  \w     84.00 148.00   1.00   17.00    --  113.00  77.00 120.00   64
  6  \w     79.00 178.00   1.00   17.00    --  113.00  77.00  90.00   99
  7  \w    -63.00  37.00   1.00    4.20    --  -40.13  77.00 -30.00  100
  8  \w    -93.00 -65.00   1.00    4.20    --  -40.13 -77.00  90.00   28
  9  \w    -98.00 -72.00   1.00    4.20    --  -40.13-139.00  44.00   26
 10  \w      4.00  79.00   1.00    4.20    --   40.13 -99.00  90.00   75
 11  \w     82.00 108.00   1.00    4.20    --   40.13  57.00 120.00   26
 12  \w    104.00 166.00   1.00   17.00    --  113.00 112.00-180.00   62
 13  \w     43.00  92.00   1.00   17.00    --  113.00 -95.00 -60.00   49
 14  \w    114.00 156.00   1.00   17.00    --  113.00 112.00-150.00   42
 15  \w    137.00 167.00   1.00   17.00    --  113.00 112.00 -90.00   30
 16  \w     43.00 101.00   1.00   17.00    --  113.00 -95.00 120.00   58
 17  \w     88.00 114.00   1.00   17.00    --  113.00  61.00-180.00   26
 18  \w    105.00 134.00   1.00   17.00    --  113.00 112.00 -90.00   29
 19  \w     44.00 107.00   1.00   17.00    --  113.00 -95.00-150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0287292000
_diffrn_orient_matrix_UB_12      0.0027666000
_diffrn_orient_matrix_UB_13      -0.0663537000
_diffrn_orient_matrix_UB_21      0.0753651000
_diffrn_orient_matrix_UB_22      0.0677554000
_diffrn_orient_matrix_UB_23      0.0178006000
_diffrn_orient_matrix_UB_31      0.0289156000
_diffrn_orient_matrix_UB_32      -0.0523287000
_diffrn_orient_matrix_UB_33      0.0194171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12896
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        64.992
_diffrn_reflns_theta_max         64.992
_diffrn_reflns_theta_min         4.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       needle
_exptl_crystal_F_000             3564
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.533
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+30.1470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2923
_reflns_number_total             3034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00892k2.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1566876
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C15 H15 I1 O3 S1'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C5(H5), C6(H6), C11(H11), C9(H9)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              81555
_shelx_hkl_checksum              59053
_shelx_fab_checksum              26748
_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 2.142
_oxdiff_exptl_absorpt_empirical_full_min 0.434