The construction of a stable hydrogen-bonded organic framework for the photocatalytic reduction and removal of uranium.
Zhang, Li; Luo, Yu-Ting; Xiao, Sai-Jin; Fan, Jia-Qi; Tan, Quan-Gen; Sun, Chen; Song, An-Min; Liang, Ru-Ping; Qiu, Jian-Ding; Chemical communications (Cambridge, England) 60 (2024) 3583–3586; doi:10.1039/d4cc00438h

data_7132802
_publ_section_title
;
 The construction of a stable hydrogen-bonded organic framework for the
 photocatalytic reduction and removal of uranium.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3583
_journal_page_last               3586
_journal_paper_doi               10.1039/d4cc00438h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H28 N8, 1[C3H7NO]'
_chemical_formula_sum            'C38 H28 N8'
_chemical_formula_weight         596.68
_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
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2024-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.722(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5521(2)
_cell_length_b                   9.4107(2)
_cell_length_c                   32.5260(6)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.6600
_cell_measurement_theta_min      2.6590
_cell_volume                     3518.39(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_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    -20.00  27.00   0.50    0.05    --  -48.70  19.00  30.00   94
  2  \w    -66.00  21.00   0.50    0.05    --  -48.70  81.00 -46.00  174
  3  \w    -61.00 -28.00   0.50    0.09    -- -101.00  61.00-150.00   66
  4  \w    -68.00 -41.00   0.50    0.09    -- -101.00  61.00 -90.00   54
  5  \w    -68.00 -32.00   0.50    0.09    -- -101.00  61.00 -60.00   72
  6  \w    -58.00 -32.00   0.50    0.09    -- -101.00  61.00  90.00   52
  7  \w   -125.00 -49.00   0.50    0.09    -- -101.00  81.00 -46.00  152
  8  \w   -168.00-113.00   0.50    0.09    -- -101.00 -15.00-120.00  110
  9  \w   -110.00 -84.00   0.50    0.09    -- -101.00 -94.00 -30.00   52
 10  \w   -115.00 -88.00   0.50    0.05    --  -48.70-125.00 -30.00   54
 11  \w   -106.00 -78.00   0.50    0.05    --  -48.70-125.00   0.00   56
 12  \w   -120.00 -77.00   0.50    0.05    --  -48.70-125.00 -90.00   86
 13  \w     -7.00  71.00   0.50    0.05    --   48.70 -81.00-169.00  156
 14  \w     36.00  71.00   0.50    0.09    --  103.25 -81.00-169.00   70
 15  \w     31.00 111.00   0.50    0.09    --  103.25-125.00-180.00  160
 16  \w     37.00  62.00   0.50    0.09    --  103.25 -61.00 -30.00   50
 17  \w     32.00  57.00   0.50    0.09    --  103.25 -61.00   0.00   50
 18  \w     50.00  75.00   0.50    0.09    --  103.25 -61.00  60.00   50
 19  \w     92.00 178.00   0.50    0.09    --  103.25  30.00  60.00  172
 20  \w    107.00 132.00   0.50    0.09    --  103.25  81.00 -46.00   50
 21  \w    145.00 175.00   0.50    0.09    --  103.25  30.00 -90.00   60
 22  \w    102.00 127.00   0.50    0.09    --  103.25  30.00 -90.00   50
 23  \w   -173.00 -97.00   0.50    0.09    -- -101.00 -81.00-169.00  152
 24  \w   -172.00-144.00   0.50    0.09    -- -101.00 -94.00 -30.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0232198000
_diffrn_orient_matrix_UB_12      -0.0443119000
_diffrn_orient_matrix_UB_13      -0.0440168000
_diffrn_orient_matrix_UB_21      0.0634302000
_diffrn_orient_matrix_UB_22      -0.1342648000
_diffrn_orient_matrix_UB_23      0.0174496000
_diffrn_orient_matrix_UB_31      -0.1157858000
_diffrn_orient_matrix_UB_32      -0.0825439000
_diffrn_orient_matrix_UB_33      -0.0047666000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.963
_diffrn_reflns_theta_min         2.731
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.126
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1156P)^2^+0.5516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5342
_reflns_number_total             6993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00438h2.cif
_cod_data_source_block           lyt20230323-hof
_cod_depositor_comments          'Adding full bibliography for 7132802.cif.'
_cod_database_code               7132802
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C20(H20), C19(H19), C10(H10), C17(H17), C6(H6), C2(H2), C11(H11),
 C5(H5), C3(H3), C14(H14), C13(H13), C33(H33), C26(H26), C36(H36), C22(H22),
 C25(H25), C23(H23), C43(H43), C38(H38), C35(H35), C39(H39), C46(H46), C44(H44),
  C30(H30), C41(H41), C28(H28), C31(H31)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18443
_shelx_hkl_checksum              72433
_shelx_fab_checksum              67514
_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 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.471