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_7134726
_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         'C108 H84 Eu2 N2 O20'
_chemical_formula_sum            'C108 H84 Eu2 N2 O20'
_chemical_formula_weight         2033.69
_chemical_melting_point          100
_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             2025-02-15
_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                91.069(2)
_cell_angle_beta                 94.535(2)
_cell_angle_gamma                103.539(3)
_cell_formula_units_Z            1
_cell_length_a                   11.8861(4)
_cell_length_b                   15.3328(5)
_cell_length_c                   19.6363(3)
_cell_measurement_reflns_used    15087
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5110
_cell_measurement_theta_min      2.2650
_cell_volume                     3465.77(18)
_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 2014/5 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.954
_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   -119.00 -38.00   0.50    1.00    --  -47.65 -56.00   2.00  162
  2  \w    -29.00  25.00   0.50    1.00    --  -47.65  56.00 144.00  108
  3  \w     46.00 116.00   0.50    1.00    --   47.65  56.00 144.00  140
  4  \w    -24.00  60.00   0.50    1.00    --   47.65 -56.00   2.00  168
  5  \w   -173.00-113.00   0.50    9.50    -- -104.50 -56.00   2.00  120
  6  \w    -60.00 -34.00   0.50    9.50    -- -104.50  56.00 144.00   52
  7  \w    100.00 178.00   0.50    9.50    --  106.54  56.00 144.00  156
  8  \w     34.00  67.00   0.50    9.50    --  106.54 -56.00   2.00   66
  9  \w     -6.00  20.00   0.50    1.00    --  -47.65  77.00-120.00   52
 10  \w    -67.00 -32.00   0.50    1.00    --  -47.65  77.00-120.00   70
 11  \w    -23.00   6.00   0.50    1.00    --  -47.65  19.00 150.00   58
 12  \w    -15.00  22.00   0.50    1.00    --  -47.65  19.00  90.00   74
 13  \w     -3.00  27.00   0.50    1.00    --  -47.65  19.00 -60.00   60
 14  \w     28.00  86.00   0.50    1.00    --   47.65-125.00-120.00  116
 15  \w   -129.00-103.00   0.50    9.50    -- -104.50 149.00-169.13   52
 16  \w   -167.00-131.00   0.50    9.50    -- -104.50 -15.00 -30.00   72
 17  \w    -63.00 -34.00   0.50    9.50    -- -104.50  61.00-120.00   58
 18  \w   -105.00 -78.00   0.50    9.50    -- -104.50 125.00 150.00   54
 19  \w    -70.00 -35.00   0.50    9.50    -- -104.50 125.00 150.00   70
 20  \w   -144.00 -92.00   0.50    9.50    -- -104.50 -45.00-120.00  104
 21  \w    -66.00 -39.00   0.50    9.50    -- -104.50  61.00 -60.00   54
 22  \w    -71.00 -32.00   0.50    9.50    -- -104.50 149.00-169.13   78
 23  \w    -61.00 -34.00   0.50    9.50    -- -104.50  77.00-180.00   54
 24  \w    -99.00 -32.00   0.50    9.50    -- -104.50  77.00 -60.00  134
 25  \w   -119.00 -93.00   0.50    9.50    -- -104.50 136.00  13.05   52
 26  \w    -98.00 -71.00   0.50    9.50    -- -104.50  77.00-180.00   54
 27  \w   -173.00-111.00   0.50    9.50    -- -104.50 -45.00  60.00  124
 28  \w    -96.00 -40.00   0.50    9.50    -- -104.50  77.00  30.00  112
 29  \w   -126.00 -32.00   0.50    9.50    -- -104.50 145.00  36.06  188
 30  \w   -107.00 -76.00   0.50    9.50    -- -104.50 109.00 -63.22   62
 31  \w   -118.00 -93.00   0.50    9.50    -- -104.50 -15.00 -30.00   50
 32  \w     60.00 105.00   0.50    9.50    --  106.54-125.00  60.00   90
 33  \w     77.00 108.00   0.50    9.50    --  106.54-109.00-161.68   62
 34  \w    132.00 167.00   0.50    9.50    --  106.54  61.00  60.00   70
 35  \w     68.00 104.00   0.50    9.50    --  106.54 -77.00 120.00   72
 36  \w     34.00  63.00   0.50    9.50    --  106.54 -77.00 120.00   58
 37  \w     81.00 174.00   0.50    9.50    --  106.54 125.00  60.00  186
 38  \w     67.00 104.00   0.50    9.50    --  106.54 -95.00 120.00   74
 39  \w    150.00 178.00   0.50    9.50    --  106.54  45.00-150.00   56
 40  \w    107.00 143.00   0.50    9.50    --  106.54  45.00-150.00   72
 41  \w     37.00 111.00   0.50    9.50    --  106.54-125.00  90.00  148
 42  \w     59.00  98.00   0.50    9.50    --  106.54 -95.00-120.00   78
 43  \w     39.00  85.00   0.50    9.50    --  106.54 -77.00 -30.00   92
 44  \w     50.00  75.00   0.50    9.50    --  106.54 -61.00-180.00   50
 45  \w     37.00  62.00   0.50    9.50    --  106.54 -95.00 -30.00   50
 46  \w     99.00 126.00   0.50    9.50    --  106.54  61.00  60.00   54
;
_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      -0.0256880000
_diffrn_orient_matrix_UB_12      0.0918350000
_diffrn_orient_matrix_UB_13      -0.0156760000
_diffrn_orient_matrix_UB_21      -0.1025744000
_diffrn_orient_matrix_UB_22      -0.0463529000
_diffrn_orient_matrix_UB_23      -0.0511198000
_diffrn_orient_matrix_UB_31      -0.0819964000
_diffrn_orient_matrix_UB_32      -0.0106765000
_diffrn_orient_matrix_UB_33      0.0578275000
_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  0.1461
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.223
_diffrn_reflns_theta_min         2.259
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74219
_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    0.974
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_refine_diff_density_max         2.008
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         14016
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.1121
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3030
_refine_ls_wR_factor_ref         0.3299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9745
_reflns_number_total             14016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02537k2.cif
_cod_data_source_block           NKM-567-Eu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '100 K' was changed to
'100' -- the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134726--7134728.cif.
;
_cod_database_code               7134726
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Eu'
_chemical_oxdiff_usercomment     'C H O N Eu'
_olex2_refinement_description
;
1. Restrained distances
 C46-O9
 1.44 with sigma of 0.02
 C46-C47
 1.5 with sigma of 0.02
 C47-C48
 1.5 with sigma of 0.02
 C48-C49
 1.5 with sigma of 0.02
 C44-C46
 2.4 with sigma of 0.02
 O9-C47
 2.4 with sigma of 0.02
 C46-C48
 2.5 with sigma of 0.02
 C47-C49
 2.5 with sigma of 0.02
 C53-N1
 1.45 with sigma of 0.02
 N1-C51
 1.45 with sigma of 0.02
 C53-C54
 1.5 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C54-N1
 2.53 with sigma of 0.02
 N1-C52
 2.53 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C49) = Uanis(C48) = Uanis(C47) = Uanis(C46) = Uanis(O9) = Uanis(C44) =
Uanis(C45) = Uanis(C43)
Uanis(C52) = Uanis(C51) = Uanis(N1) = Uanis(C50) = Uanis(C53) = Uanis(C54) =
Uanis(O10)
Uanis(O6) = Uanis(C39) = Uanis(O5)
3.a Ternary CH refined with riding coordinates:
 C42(H42), C21(H21)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C51(H51A,H51B), C53(H53A,H53B), C48(H48A,H48B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C17(H17), C24(H24), C4(H4), C7(H7), C27(H27), C3(H3), C6(H6),
 C33(H33), C34(H34), C11(H11), C30(H30), C12(H12), C15(H15), C29(H29), C36(H36),
  C41(H41), C14(H14), C37(H37), C40(H40), C50(H50)
3.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C49(H49A,H49B,H49C), C54(H54A,H54B,H54C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10097
_shelx_hkl_checksum              80967
_shelx_fab_checksum              77092
_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 2.247
_oxdiff_exptl_absorpt_empirical_full_min 0.485