Rare-earth-pentacene-octacarboxylate frameworks for highly efficient urinary 1-HP fluorescence sensing.
Zhang, Jinli; Xi, Xiao-Juan; Xu, Lin; Lang, Feifan; Yang, Yan; Pang, Jiandong; Chemical communications (Cambridge, England) 61 (2025) 11195–11198; doi:10.1039/d5cc02537k

data_7134728
_publ_section_title
;
 Rare-earth-pentacene-octacarboxylate frameworks for highly efficient
 urinary 1-HP fluorescence sensing.
;
_journal_issue                   60
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11195
_journal_page_last               11198
_journal_paper_doi               10.1039/d5cc02537k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C105.1 H75.9 N2 O19.6 Tb2'
_chemical_formula_sum            'C105.1 H75.9 N2 O19.6 Tb2'
_chemical_formula_weight         1998.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-05-03 deposited with the CCDC.	2025-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                91.859(3)
_cell_angle_beta                 94.475(3)
_cell_angle_gamma                103.284(4)
_cell_formula_units_Z            1
_cell_length_a                   11.7036(5)
_cell_length_b                   15.2043(7)
_cell_length_c                   19.7918(7)
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3240
_cell_measurement_theta_min      2.9900
_cell_volume                     3412.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.962
_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    -24.00  68.00   0.50    0.21    --   47.66 -71.00 113.00  184
  2  \w     73.00  99.00   0.50    0.83    --  106.53 -77.00 -90.00   52
  3  \w     36.00  72.00   0.50    0.83    --  106.53 -77.00 -90.00   72
  4  \w     35.00  74.00   0.50    0.83    --  106.53 -61.00 -90.00   78
  5  \w     21.00  46.00   0.50    0.21    --   47.66 -38.00 -90.00   50
  6  \w     28.00 119.00   0.50    0.21    --   47.66  71.00-115.00  182
  7  \w    132.00 159.00   0.50    0.83    --  106.53  71.00-115.00   54
  8  \w    150.00 177.00   0.50    0.83    --  106.53  15.00-180.00   54
  9  \w     94.00 127.00   0.50    0.83    --  106.53  15.00-180.00   66
 10  \w     47.00  88.00   0.50    0.83    --  106.53 -95.00  30.00   82
 11  \w      0.00  27.00   0.50    0.21    --  -47.66  19.00-120.00   54
 12  \w    -68.00  25.00   0.50    0.21    --  -47.66  71.00-115.00  186
 13  \w    -21.00  20.00   0.50    0.21    --  -47.66  19.00  60.00   82
 14  \w    -66.00 -41.00   0.50    0.83    -- -104.50  61.00  30.00   50
 15  \w    -80.00 -43.00   0.50    0.83    -- -104.50  71.00-115.00   74
 16  \w    -58.00 -33.00   0.50    0.83    -- -104.50  61.00-120.00   50
 17  \w   -174.00 -87.00   0.50    0.83    -- -104.50 -71.00 113.00  174
 18  \w   -123.00 -98.00   0.50    0.83    -- -104.50 -15.00 150.00   50
 19  \w   -173.00-140.00   0.50    0.83    -- -104.50 -15.00 150.00   66
 20  \w     73.00 100.00   0.50    0.86    --  106.53 -77.00 -90.00   54
 21  \w     43.00  72.00   0.50    0.86    --  106.53 -77.00 -90.00   58
 22  \w     34.00  73.00   0.50    0.86    --  106.53 -61.00 -90.00   78
 23  \w    -12.00  16.00   0.50    0.22    --   47.66 -71.00 113.00   56
 24  \w     39.00  64.00   0.50    0.86    --  106.53 -71.00 113.00   50
 25  \w      1.00  26.00   0.50    0.22    --   47.66 -38.00 -90.00   50
 26  \w     55.00 119.00   0.50    0.22    --   47.66  71.00-115.00  128
 27  \w     88.00 171.00   0.50    0.86    --  106.53  71.00-115.00  166
 28  \w    153.00 178.00   0.50    0.86    --  106.53  15.00-180.00   50
 29  \w     96.00 122.00   0.50    0.86    --  106.53  15.00-180.00   52
 30  \w     50.00  84.00   0.50    0.86    --  106.53 -95.00  30.00   68
 31  \w    -20.00  21.00   0.50    0.22    --  -47.66  19.00  60.00   82
 32  \w    -34.00   8.00   0.50    0.22    --  -47.66  71.00-115.00   84
 33  \w     -2.00  23.00   0.50    0.22    --  -47.66  19.00-120.00   50
 34  \w    -69.00 -38.00   0.50    0.86    -- -104.50  71.00-115.00   62
 35  \w    -67.00 -32.00   0.50    0.86    -- -104.50  61.00-120.00   70
 36  \w    -65.00 -40.00   0.50    0.86    -- -104.50  61.00  30.00   50
 37  \w   -116.00 -91.00   0.50    0.86    -- -104.50 -15.00 150.00   50
 38  \w   -173.00-131.00   0.50    0.86    -- -104.50 -15.00 150.00   84
 39  \w   -169.00-142.00   0.50    0.86    -- -104.50 -71.00 113.00   54
 40  \w    -61.00 -32.00   0.50    0.87    -- -104.50  61.00  60.00   58
 41  \w    -65.00 -39.00   0.50    0.87    -- -104.50  61.00  30.00   52
 42  \w    -58.00 -32.00   0.50    0.87    -- -104.50  61.00   0.00   52
 43  \w    -22.00  28.00   0.50    0.22    --  -47.66  17.00  94.00  100
 44  \w    -68.00 -36.00   0.50    0.87    -- -104.50  61.00 -60.00   64
 45  \w    -67.00 -41.00   0.50    0.87    -- -104.50  61.00 -90.00   52
 46  \w   -119.00 -91.00   0.50    0.87    -- -104.50 -17.00 -73.00   56
 47  \w   -122.00 -34.00   0.50    0.22    --  -47.66 -17.00 -73.00  176
 48  \w     55.00 102.00   0.50    0.22    --   47.66  17.00  94.00   94
 49  \w     95.00 178.00   0.50    0.87    --  106.53  17.00  94.00  166
 50  \w     35.00 106.00   0.50    0.87    --  106.53 -77.00 -30.00  142
 51  \w     34.00  59.00   0.50    0.87    --  106.53 -61.00 -30.00   50
 52  \w    -26.00  29.00   0.50    0.22    --   47.66 -17.00 -73.00  110
 53  \w     58.00 101.00   0.50    0.87    --  106.53 -77.00-180.00   86
 54  \w     39.00  95.00   0.50    0.87    --  106.53-125.00-180.00  112
 55  \w     56.00 107.00   0.50    0.87    --  106.53-125.00-150.00  102
 56  \w     20.00  90.00   0.50    0.22    --   47.66-125.00-180.00  140
 57  \w    -68.00 -43.00   0.50    1.04    -- -104.50  61.00-120.00   50
 58  \w    -66.00 -38.00   0.50    1.04    -- -104.50  61.00 -90.00   56
 59  \w    -67.00 -37.00   0.50    1.04    -- -104.50  61.00 -60.00   60
 60  \w    -58.00 -32.00   0.50    1.04    -- -104.50  61.00   0.00   52
 61  \w    -22.00  28.00   0.50    0.26    --  -47.66  17.00  95.00  100
 62  \w    -64.00 -38.00   0.50    1.04    -- -104.50  61.00  30.00   52
 63  \w   -173.00 -96.00   0.50    1.04    -- -104.50 -17.00 -73.00  154
 64  \w   -122.00 -34.00   0.50    0.26    --  -47.66 -17.00 -73.00  176
 65  \w     20.00  89.00   0.50    0.26    --   47.66-125.00-180.00  138
 66  \w     37.00  63.00   0.50    1.04    --  106.53-125.00-180.00   52
 67  \w     84.00 111.00   0.50    1.04    --  106.53-125.00-180.00   54
 68  \w     80.00 105.00   0.50    1.04    --  106.53 -95.00-150.00   50
 69  \w     34.00  61.00   0.50    1.04    --  106.53 -95.00-150.00   54
 70  \w    -27.00  29.00   0.50    0.26    --   47.66 -17.00 -73.00  112
 71  \w     38.00  64.00   0.50    1.04    --  106.53 -61.00 -30.00   52
 72  \w     34.00  66.00   0.50    1.04    --  106.53 -77.00 120.00   64
 73  \w     68.00  94.00   0.50    1.04    --  106.53 -77.00 120.00   52
 74  \w    111.00 136.00   0.50    1.04    --  106.53  17.00  95.00   50
 75  \w    150.00 176.00   0.50    1.04    --  106.53 125.00 -90.00   52
 76  \w     80.00 106.00   0.50    1.04    --  106.53 125.00 -90.00   52
 77  \w     35.00 118.00   0.50    0.26    --   47.66  17.00  95.00  166
;
_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      0.0701350000
_diffrn_orient_matrix_UB_12      0.0452855000
_diffrn_orient_matrix_UB_13      -0.0573660000
_diffrn_orient_matrix_UB_21      0.0736755000
_diffrn_orient_matrix_UB_22      -0.0719575000
_diffrn_orient_matrix_UB_23      0.0025020000
_diffrn_orient_matrix_UB_31      -0.0899324000
_diffrn_orient_matrix_UB_32      -0.0603278000
_diffrn_orient_matrix_UB_33      -0.0530595000
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65840
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.427
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_description       needle
_exptl_crystal_F_000             1007
_refine_diff_density_max         2.295
_refine_diff_density_min         -4.810
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         11720
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1576P)^2^+38.7992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10923
_reflns_number_total             11720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02537k2.cif
_cod_data_source_block           NKM-567-Tb
_cod_depositor_comments
'Adding full bibliography for 7134726--7134728.cif.'
_cod_original_formula_sum        'C105.10 H75.90 N2 O19.60 Tb2'
_cod_database_code               7134728
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O Tb'
_olex2_refinement_description
;
1. Restrained distances
 O10-C50
 1.26 with sigma of 0.02
 C50-N1
 1.33 with sigma of 0.02
 N1-C51
 1.48 with sigma of 0.02
 N1-C53
 1.48 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C53-C54
 1.5 with sigma of 0.02
 C52-N1
 2.5 with sigma of 0.02
 N1-C54
 2.5 with sigma of 0.02
 C24-O5
 1.37 with sigma of 0.02
 C25-O5
 1.44 with sigma of 0.02
 C25-C26
 1.5 with sigma of 0.02
 C26-C27
 1.5 with sigma of 0.02
 C27-C28
 1.5 with sigma of 0.02
 C24-C25
 2.4 with sigma of 0.02
 O5-C26
 2.4 with sigma of 0.02
 C25-C27
 2.5 with sigma of 0.02
 C26-C28
 2.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(O5) = Uanis(C24) =
Uanis(C23) = Uanis(C22)
Uanis(O7) = Uanis(C40) = Uanis(O6) = Uanis(C39)
Uanis(O4) = Uanis(C14) = Uanis(O3) = Uanis(C13)
Uanis(C52) = Uanis(C51) = Uanis(N1) = Uanis(C53) = Uanis(C54) = Uanis(C50) =
Uanis(O10)
3. Others
 Fixed Sof: O7(0.8) C26(0.7) H26A(0.7) H26B(0.7) C54(0.6) H54C(0.6) H54A(0.6)
 H54B(0.6) C52(0.25) H52A(0.25) H52B(0.25) H52C(0.25)
4.a Ternary CH refined with riding coordinates:
 C21(H21), C29(H29)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C51(H51A,H51B), C53(H53B,H53A), C26(H26A,H26B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C3(H3), C17(H17), C35(H35), C4(H4), C32(H32), C7(H7), C49(H49),
 C6(H6), C11(H11), C44(H44), C42(H42), C48(H48), C45(H45), C37(H37), C12(H12),
 C16(H16), C15(H15), C38(H38), C41(H41), C50(H50)
4.d Idealised Me refined as rotating group:
 C54(H54C,H54A,H54B), C52(H52A,H52B,H52C), C28(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3992
_shelx_hkl_checksum              39745
_shelx_fab_checksum              84715
_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 1.419
_oxdiff_exptl_absorpt_empirical_full_min 0.245