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_7134727
_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         'C107 H81 Ce2 N2 O20'
_chemical_formula_sum            'C107 H81 Ce2 N2 O20'
_chemical_formula_weight         1994.97
_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                91.6820(10)
_cell_angle_beta                 94.913(2)
_cell_angle_gamma                102.427(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0155(3)
_cell_length_b                   15.2802(2)
_cell_length_c                   19.6685(3)
_cell_measurement_reflns_used    39192
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7890
_cell_measurement_theta_min      2.9790
_cell_volume                     3509.32(12)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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     19.00  93.00   0.50    0.05    --   47.66-125.00  90.00  148
  2  \w     36.00 107.00   0.50    0.13    --  105.90-125.00 120.00  142
  3  \w     69.00 102.00   0.50    0.13    --  105.90 -95.00  90.00   66
  4  \w     39.00 104.00   0.50    0.13    --  105.90 -95.00 150.00  130
  5  \w     71.00 103.00   0.50    0.13    --  105.90 -95.00   0.00   64
  6  \w     86.00 112.00   0.50    0.13    --  105.90-125.00 -60.00   52
  7  \w     40.00  90.00   0.50    0.13    --  105.90 -95.00-120.00  100
  8  \w     42.00  75.00   0.50    0.13    --  105.90 -61.00 -30.00   66
  9  \w     44.00  73.00   0.50    0.13    --  105.90 -61.00 -90.00   58
 10  \w     39.00  65.00   0.50    0.13    --  105.90 -61.00  30.00   52
 11  \w    -24.00  70.00   0.50    0.05    --   47.66 -77.00 132.00  188
 12  \w     33.00 108.00   0.50    0.13    --  105.90 -77.00 132.00  150
 13  \w     33.00  75.00   0.50    0.13    --  105.90 -61.00  90.00   84
 14  \w    109.00 135.00   0.50    0.13    --  105.90  15.00 120.00   52
 15  \w    145.00 170.00   0.50    0.13    --  105.90  15.00 120.00   50
 16  \w     83.00 178.00   0.50    0.13    --  105.90  77.00-101.00  190
 17  \w     93.00 178.00   0.50    0.13    --  105.90  45.00-150.00  170
 18  \w     93.00 157.00   0.50    0.13    --  105.90  30.00-180.00  128
 19  \w     25.00 119.00   0.50    0.05    --   47.66  77.00-101.00  188
 20  \w    -70.00  25.00   0.50    0.05    --  -47.66  77.00-101.00  190
 21  \w    -23.00  28.00   0.50    0.05    --  -47.66  19.00 -90.00  102
 22  \w    -39.00  25.00   0.50    0.05    --  -47.66  38.00-120.00  128
 23  \w    -23.00  28.00   0.50    0.05    --  -47.66  19.00-150.00  102
 24  \w    -23.00  28.00   0.50    0.05    --  -47.66  19.00 -30.00  102
 25  \w    -23.00  28.00   0.50    0.05    --  -47.66  19.00  60.00  102
 26  \w   -108.00 -35.00   0.50    0.13    -- -104.50 110.00  69.40  146
 27  \w   -123.00 -32.00   0.50    0.13    -- -104.50 140.00 135.44  182
 28  \w   -111.00 -35.00   0.50    0.13    -- -104.50 125.00 -60.00  152
 29  \w   -111.00 -35.00   0.50    0.13    -- -104.50 125.00 -90.00  152
 30  \w   -111.00 -35.00   0.50    0.13    -- -104.50 125.00-150.00  152
 31  \w   -123.00 -32.00   0.50    0.13    -- -104.50 140.00-104.33  182
 32  \w   -111.00 -35.00   0.50    0.13    -- -104.50 125.00   0.00  152
 33  \w    -68.00 -32.00   0.50    0.13    -- -104.50  61.00  30.00   72
 34  \w    -68.00 -32.00   0.50    0.13    -- -104.50  61.00  90.00   72
 35  \w    -68.00 -32.00   0.50    0.13    -- -104.50  61.00 150.00   72
 36  \w   -101.00 -32.00   0.50    0.13    -- -104.50  77.00   0.00  138
 37  \w   -101.00 -32.00   0.50    0.13    -- -104.50  77.00 -30.00  138
 38  \w   -101.00 -32.00   0.50    0.13    -- -104.50  77.00-101.00  138
 39  \w   -174.00 -91.00   0.50    0.13    -- -104.50 -51.00-148.29  166
 40  \w   -174.00 -89.00   0.50    0.13    -- -104.50 -58.00-109.28  170
 41  \w   -174.00 -90.00   0.50    0.13    -- -104.50 -56.00-119.65  168
 42  \w   -174.00 -90.00   0.50    0.13    -- -104.50 -56.00-179.84  168
 43  \w   -119.00 -25.00   0.50    0.05    --  -47.66 -77.00 132.00  188
 44  \w   -174.00 -82.00   0.50    0.13    -- -104.50 -77.00 132.00  184
;
_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      0.0741273000
_diffrn_orient_matrix_UB_12      0.0483512000
_diffrn_orient_matrix_UB_13      0.0635444000
_diffrn_orient_matrix_UB_21      -0.0983709000
_diffrn_orient_matrix_UB_22      0.0443903000
_diffrn_orient_matrix_UB_23      0.0173083000
_diffrn_orient_matrix_UB_31      -0.0471152000
_diffrn_orient_matrix_UB_32      -0.0798483000
_diffrn_orient_matrix_UB_33      0.0431005000
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.837
_diffrn_reflns_theta_min         2.257
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61866
_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    0.944
_exptl_crystal_description       needle
_exptl_crystal_F_000             1013
_refine_diff_density_max         2.693
_refine_diff_density_min         -3.616
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         14357
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1632P)^2^+14.4404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13362
_reflns_number_total             14357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02537k2.cif
_cod_data_source_block           NKM-567-Ce
_cod_depositor_comments
'Adding full bibliography for 7134726--7134728.cif.'
_cod_database_code               7134727
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O Ce'
_olex2_refinement_description
;
1. Restrained distances
 C23-O5
 1.37 with sigma of 0.02
 O5-C25
 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
 C23-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
 2.55 with sigma of 0.02
 O10-C50
 1.26 with sigma of 0.02
 C50-N1
 1.33 with sigma of 0.02
 C51-N1
 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
2. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(O5) = Uanis(C23) =
Uanis(C24) = Uanis(C22)
Uanis(O6) = Uanis(C38) = Uanis(O7)
Uanis(O3) = Uanis(C14) = Uanis(O4) = Uanis(C13)
Uanis(C52) = Uanis(C51) = Uanis(N1) = Uanis(C53) = Uanis(C54) = Uanis(C50) =
Uanis(O10)
3. Others
 Fixed Sof: C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
4.a Ternary CH refined with riding coordinates:
 C29(H29), C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C51(H51A,H51B), C53(H53A,H53B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C32(H32), C42(H42), C40(H40), C7(H7), C3(H3), C4(H4),
 C6(H6), C44(H44), C12(H12), C48(H48), C45(H45), C39(H39), C11(H11), C35(H35),
 C36(H36), C49(H49), C16(H16), C15(H15), C50(H50)
4.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24879
_shelx_hkl_checksum              49043
_shelx_fab_checksum              81538
_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 2.050
_oxdiff_exptl_absorpt_empirical_full_min 0.415