Tailoring Exciplex Formation in Metal-Induced Supramolecular Organization
Le-Hoang, Giau; Guénée, Laure; Piguet, Claude; Dalton Transactions  (2026) –; doi:10.1039/D6DT00490C

data_7720826
_publ_section_title
;
 Tailoring Exciplex Formation in Metal-Induced Supramolecular Organization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00490C
_journal_year                    2026
_chemical_formula_moiety         'C64 H52 Eu F18 N5 O7'
_chemical_formula_sum            'C64 H52 Eu F18 N5 O7'
_chemical_formula_weight         1497.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-08-20
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-17 deposited with the CCDC.	2026-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6632(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.92754(11)
_cell_length_b                   16.67760(8)
_cell_length_c                   16.28183(7)
_cell_measurement_reflns_used    50837
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      75.8110
_cell_measurement_theta_min      3.2710
_cell_volume                     6170.18(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (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 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -78.00 -52.00   0.50    4.00    --  -57.24 112.00  43.00   52
  2  \w    -47.00 -18.00   0.50    4.00    --  -57.24 112.00  43.00   58
  3  \w     20.00  45.00   0.50    4.00    --   60.05 -94.00  60.00   50
  4  \w     20.00  47.00   0.50    4.00    --   60.05 -94.00 150.00   54
  5  \w     52.00 104.00   0.50    4.00    --   60.05  15.00  30.00  104
  6  \w     75.00 103.00   0.50    4.00    --   60.05  15.00 150.00   56
  7  \w     82.00 107.00   0.50    4.00    --   60.05  15.00 -90.00   50
  8  \w     23.00  60.00   0.50    4.00    --   60.05 -94.00  30.00   74
  9  \w     30.00  63.00   0.50    4.00    --   60.05  15.00 -90.00   66
 10  \w     27.00  70.00   0.50    4.00    --   60.05 -94.00 -60.00   86
 11  \w     45.00  87.00   0.50    4.00    --   60.05  15.00  90.00   84
 12  \w     28.00  71.00   0.50    4.00    --   60.05  15.00 150.00   86
 13  \w     26.00  60.00   0.50    4.00    --   60.05 -94.00  90.00   68
 14  \w    -71.00 -46.00   0.50    4.00    --  -64.50 -22.00-158.51   50
 15  \w    -56.00 -30.00   0.50    4.00    --  -64.50  84.00 146.67   52
 16  \w    -60.00 -35.00   0.50    4.00    --  -64.50  74.00 126.97   50
 17  \w   -111.00 -39.00   0.50    4.00    --  -64.50 -20.00 169.34  144
 18  \w     40.00  66.00   0.50    4.00    --   74.47 -94.00 -30.00   52
 19  \w     38.00  70.00   0.50    4.00    --   74.47 -94.00  30.00   64
 20  \w     35.00  61.00   0.50    4.00    --   74.47 -94.00-150.00   52
 21  \w     76.00 102.00   0.50    4.00    --   74.47-125.00-150.00   52
 22  \w     39.00  65.00   0.50    4.00    --   74.47-125.00-150.00   52
 23  \w     35.00 103.00   0.50    4.00    --   74.47-125.00 -60.00  136
 24  \w     75.00 122.00   0.50    4.00    --   74.47  15.00-180.00   94
 25  \w     46.00  73.00   0.50    4.00    --   79.86 -94.00  90.00   54
 26  \w     41.00  69.00   0.50    4.00    --   79.86 -94.00  60.00   56
 27  \w     60.00  88.00   0.50    4.00    --   79.86 -94.00 -30.00   56
 28  \w     42.00  68.00   0.50    4.00    --   79.86 -94.00 150.00   52
 29  \w     39.00  94.00   0.50    4.00    --   79.86-125.00 -60.00  110
 30  \w     47.00  74.00   0.50    4.00    --   79.86 -94.00   0.00   54
 31  \w     92.00 127.00   0.50    4.00    --   79.86  15.00 150.00   70
 32  \w     81.00 109.00   0.50    4.00    --   79.86-125.00-180.00   56
 33  \w     55.00 122.00   0.50    4.00    --   79.86  15.00 120.00  134
 34  \w     38.00  63.00   0.50    4.00    --   79.86-125.00-180.00   50
 35  \w     40.00  94.00   0.50    4.00    --   79.86-125.00 150.00  108
 36  \w     37.00  91.00   0.50    4.00    --   79.86-125.00-120.00  108
 37  \w     73.00  98.00   0.50    4.00    --   79.86-156.00-109.00   50
 38  \w     39.00  65.00   0.50    4.00    --   79.86-125.00 120.00   52
 39  \w     38.00  94.00   0.50    4.00    --   79.86-125.00 -30.00  112
 40  \w     96.00 123.00   0.50    4.00    --   79.86  15.00 -90.00   54
 41  \w     51.00  91.00   0.50    4.00    --   79.86  15.00 -90.00   80
 42  \w     78.00 104.00   0.50    4.00    --   79.86-125.00  90.00   52
 43  \w     43.00  76.00   0.50    4.00    --   79.86 -94.00  30.00   66
 44  \w     52.00  78.00   0.50    4.00    --   79.86 -94.00-120.00   52
 45  \w     49.00 105.00   0.50    4.00    --   79.86-125.00-150.00  112
 46  \w     36.00  69.00   0.50    4.00    --   79.86-125.00 -90.00   66
 47  \w     36.00  66.00   0.50    4.00    --   79.86-125.00  90.00   60
 48  \w     54.00  80.00   0.50    4.00    --   79.86  15.00  90.00   52
 49  \w     36.00  80.00   0.50    4.00    --   79.86-125.00   0.00   88
 50  \w     51.00 111.00   0.50    4.00    --   83.50  18.00 -53.62  120
 51  \w     49.00 122.00   0.50    4.00    --   83.50  18.00  15.22  146
 52  \w     68.00 123.00   0.50    4.00    --   83.50   3.00  76.07  110
 53  \w     81.00 113.00   0.50    4.00    --   83.50-127.00  43.87   64
 54  \w     85.00 110.00   0.50    4.00    --   83.50-121.00 -49.18   50
 55  \w     39.00  65.00   0.50    4.00    --   83.50-127.00  43.87   52
 56  \w     45.00 119.00   0.50    4.00    --   83.50-135.00 -93.96  148
 57  \w     94.00 122.00   0.50    4.00    --   83.50-139.00 143.75   56
 58  \w     45.00  70.00   0.50    4.00    --   83.50-139.00 143.75   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0664572000
_diffrn_orient_matrix_UB_12      -0.0023415000
_diffrn_orient_matrix_UB_13      -0.0060911000
_diffrn_orient_matrix_UB_21      -0.0033770000
_diffrn_orient_matrix_UB_22      -0.0915736000
_diffrn_orient_matrix_UB_23      -0.0119878000
_diffrn_orient_matrix_UB_31      -0.0129695000
_diffrn_orient_matrix_UB_32      0.0117740000
_diffrn_orient_matrix_UB_33      -0.0945377000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            112105
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.000
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.281
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         12629
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0468P)^2^+11.9606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11224
_reflns_number_total             12629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00490c2.cif
_cod_data_source_block           L2Eu
_cod_database_code               7720826
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H52 N5 O7 F18 Eu1 '
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.064
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F3B \\sim F3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(F2A) \\sim Ueq, Uanis(F2B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F3A) \\sim Ueq, Uanis(F3B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C10A(H10A), C10B(H10B), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C25(H25A,H25B), C26(H26A,H26B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C16(H16), C20(H20), C21(H21),
 C22(H22), C23(H23), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42),
  C43(H43), C45(H45), C46(H46), C52(H52), C57(H57), C62(H62)
4.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C11B(H11D,H11E,H11F), C12B(H12D,
 H12E,H12F), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              826
_shelx_hkl_checksum              50047
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.424