Highly efficient iodine uptake and iodate selective probe in a 3D honeycomb-like copper–organic framework based on in situ ligand transformation
Dai, Wen; Zhang, Chuanming; Yang, Xiaoang; Li, Lincai; CrystEngComm 26 (2024) 773–782; doi:10.1039/D3CE01169K

data_7247888
_publ_section_title
;
 Highly efficient iodine uptake and iodate selective probe in a 3D
 honeycomb-like copper--organic framework based on in situ ligand
 transformation
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              773
_journal_page_last               782
_journal_paper_doi               10.1039/D3CE01169K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '0.17(C120 H72 Cu6 N24 O42), 2(O)'
_chemical_formula_sum            'C20 H18 Cu N4 O9'
_chemical_formula_weight         521.92
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-08-25 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.8181(8)
_cell_length_b                   18.8181(8)
_cell_length_c                   23.6351(7)
_cell_measurement_reflns_used    6960
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3430
_cell_measurement_theta_min      4.6100
_cell_volume                     7248.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_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    -32.00  -2.00   1.00   20.23    --  -40.45 125.00 -60.00   30
  2  \w    -65.00  29.00   1.00   20.23    --  -40.45  38.00-120.00   94
  3  \w    132.00 172.00   1.00   20.23    --  103.24 125.00   0.00   40
  4  \w    109.00 165.00   1.00   20.23    --  103.24 112.00-107.00   56
  5  \w     75.00 175.00   1.00   20.23    --  103.24  61.00-180.00  100
  6  \w    142.00 173.00   1.00   20.23    --  103.24 126.00 -97.00   31
  7  \w    127.00 155.00   1.00   20.23    --  103.24  45.00 150.00   28
  8  \w     94.00 129.00   1.00   20.23    --  103.24 125.00   0.00   35
;
_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      0.0712045000
_diffrn_orient_matrix_UB_12      -0.0122527000
_diffrn_orient_matrix_UB_13      -0.0197531000
_diffrn_orient_matrix_UB_21      0.0620133000
_diffrn_orient_matrix_UB_22      0.0889134000
_diffrn_orient_matrix_UB_23      0.0169861000
_diffrn_orient_matrix_UB_31      0.0058988000
_diffrn_orient_matrix_UB_32      -0.0292946000
_diffrn_orient_matrix_UB_33      0.0597830000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18325
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.733
_diffrn_reflns_theta_min         3.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.717
_exptl_crystal_description       needle
_exptl_crystal_F_000             1602
_exptl_crystal_recrystallization_method 'solvothermal reaction'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0984P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3860
_reflns_number_total             4728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01169k2.cif
_cod_data_source_block           20201225-dw1_sq
_cod_depositor_comments          'Adding full bibliography for 7247888.cif.'
_cod_original_cell_volume        7248.4(7)
_cod_database_code               7247888
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(6)
 0.14(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
C8 \\sim C3 \\sim C6 \\sim C9 \\sim C7 \\sim C11 \\sim C2 \\sim C10 \\sim C4
\\sim C5 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O1) = Uanis(O2) = Uanis(O3)
Uanis(N1) = Uanis(N2)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C7(H7), C2(H2), C10(H10), C4(H4), C5(H5), C1(H1A)
;
_shelx_res_checksum              41317
_shelx_fab_checksum              18916
_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 2.282
_oxdiff_exptl_absorpt_empirical_full_min 0.390