A novel Ln<sup>3+</sup>/Al<sup>3+</sup> metallacrown multifunctional material for latent fingerprint detection, luminescent thermometers and luminescent sensors.
Yan, Han; Calado, Claudia M. S.; Wang, Hao; Murugesu, Muralee; Sun, Wen-Bin; Chemical science 16 (2025) 4821–4830; doi:10.1039/d4sc08549c

data_1573890
_publ_section_title
;
 A novel Ln<sup>3+</sup>/Al<sup>3+</sup> metallacrown multifunctional
 material for latent fingerprint detection, luminescent thermometers and
 luminescent sensors.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4821
_journal_page_last               4830
_journal_paper_doi               10.1039/d4sc08549c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'2(C56 H46 Al4 Dy N4 Na O29), 8(C3 H7 N O), 0.25(H8 O4)'
_chemical_formula_sum            'C136 H150 Al8 Dy2 N16 Na2 O67'
_chemical_formula_weight         3667.53
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-08-13 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.1664(7)
_cell_length_b                   17.1664(7)
_cell_length_c                   15.3325(17)
_cell_measurement_reflns_used    5494
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.6450
_cell_measurement_theta_min      3.7250
_cell_volume                     4518.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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    -46.00  47.00   1.00    8.18    --   17.07 -82.00  71.00   93
  2  \w    -21.00  21.00   1.00    8.18    --  -16.76 -99.00 -60.00   42
  3  \w     62.00  89.00   1.00    8.18    --   17.07 178.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138992000
_diffrn_orient_matrix_UB_12      -0.0306576000
_diffrn_orient_matrix_UB_13      -0.0268359000
_diffrn_orient_matrix_UB_21      -0.0148094000
_diffrn_orient_matrix_UB_22      -0.0277215000
_diffrn_orient_matrix_UB_23      0.0299871000
_diffrn_orient_matrix_UB_31      -0.0360321000
_diffrn_orient_matrix_UB_32      -0.0004224000
_diffrn_orient_matrix_UB_33      -0.0227057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13411
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.977
_diffrn_reflns_theta_min         3.563
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0807P)^2^+7.1477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3335
_reflns_number_total             4327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08549c2.cif
_cod_data_source_block           754_auto
_cod_depositor_comments          'Adding full bibliography for 1573890.cif.'
_cod_database_code               1573890
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.06(3)
 -0.06(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C7-O7
 1.22 with sigma of 0.02
 C7-N2
 1.36 with sigma of 0.02
 N2-C15
 1.45 with sigma of 0.02
 N2-C2
 1.46 with sigma of 0.02
 O9-O2_$1
 2.5 with sigma of 0.02
 C7-C15
 2.46 with sigma of 0.04
 C7-C2
 2.45 with sigma of 0.04
 N2-C15 \\sim N2-C2
 with sigma of 0.02
4. Restrained planarity
 C7, O7, N2, C15, C2
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C15 \\sim C2 \\sim C7 \\sim O7 \\sim N2 \\sim C5 \\sim O8 \\sim C4 \\sim C17
\\sim C9 \\sim C11 \\sim C3 \\sim C13 \\sim O5 \\sim N1 \\sim O6: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C2 \\sim C7 \\sim O7 \\sim N2 \\sim C15: within 3A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3A
Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of
0.06
6. Rigid body (RIGU) restrains
 C5, C17, C13, C11, C9, C3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 C7, O7, N2, C15, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H2B(0.25) H2A(0.25) O9(0.125) H9A(0.125) H9B(0.125)
8.a Riding coordinates:
 C15(H15C,H15A,H15B), C2(H2C,H2D,H2E), O2(H2B,H2A), O9(H9A,H9B)
8.b Secondary CH2 refined with riding coordinates:
 O3(H3A,H3B)
8.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10A), C12(H12), C16(H16), C17(H17), C9(H9), C5(H5), C13(H13),
 C7(H7)
8.d Fitted hexagon refined as free rotating group:
 C6(C8,C10,C12,C14,C16), C17(C9,C5,C11,C3,C13)
8.e Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              1920
_shelx_hkl_checksum              67385
_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 1.085
_oxdiff_exptl_absorpt_empirical_full_min 0.925