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

data_7720828
_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 H51 F18 N5 O7 Y'
_chemical_formula_sum            'C64 H51 F18 N5 O7 Y'
_chemical_formula_weight         1433.01
_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             2025-09-29
_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                 91.0352(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.36202(19)
_cell_length_b                   27.8313(4)
_cell_length_c                   18.0883(2)
_cell_measurement_reflns_used    19535
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      73.7980
_cell_measurement_theta_min      2.8690
_cell_volume                     6222.28(15)
_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      119.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_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    -90.00 -25.00   0.50   10.00    --  -57.24 -15.00  90.00  130
  2  \w    -56.00 -24.00   0.50   10.00    --  -57.24 -15.00-150.00   64
  3  \w    -93.00 -68.00   0.50   10.00    --  -57.24 -15.00 150.00   50
  4  \w   -104.00 -32.00   0.50   10.00    --  -57.24 -15.00  30.00  144
  5  \w    -78.00 -28.00   0.50   10.00    --  -57.24 120.00-167.00  100
  6  \w    -86.00 -39.00   0.50   10.00    --  -57.24 125.00 -90.00   94
  7  \w    -64.00 -33.00   0.50   10.00    --  -57.24 -15.00 150.00   62
  8  \w     37.00  70.00   0.50   10.00    --   60.25 -94.00  60.00   66
  9  \w     37.00  70.00   0.50   10.00    --   60.25-125.00  60.00   66
 10  \w     48.00  81.00   0.50   10.00    --   74.77 -94.00 120.00   66
 11  \w     48.00  74.00   0.50   10.00    --   74.77-125.00 -60.00   52
 12  \w     73.00 100.00   0.50   10.00    --   74.77-125.00-180.00   54
 13  \w     40.00  89.00   0.50   10.00    --   79.86 -94.00 -90.00   98
 14  \w     45.00 109.00   0.50   10.00    --   79.86-125.00 120.00  128
 15  \w     45.00  71.00   0.50   10.00    --   79.86 -94.00 -30.00   52
 16  \w     55.00 109.00   0.50   10.00    --   79.86-125.00-180.00  108
 17  \w     42.00  77.00   0.50   10.00    --   79.86 -94.00 -60.00   70
 18  \w     47.00 119.00   0.50   10.00    --   79.86  15.00  60.00  144
 19  \w     47.00 108.00   0.50   10.00    --   79.86  15.00-150.00  122
 20  \w     90.00 127.00   0.50   10.00    --   79.86-153.00 -49.00   74
 21  \w     74.00 109.00   0.50   10.00    --   79.86-125.00 150.00   70
 22  \w     88.00 124.00   0.50   10.00    --   79.86  15.00  90.00   72
 23  \w     51.00  77.00   0.50   10.00    --   79.86-125.00  90.00   52
 24  \w     36.00  62.00   0.50   10.00    --   79.86-125.00 150.00   52
 25  \w     48.00 123.00   0.50   10.00    --   79.86  15.00 -90.00  150
 26  \w     50.00  75.00   0.50   10.00    --   79.86 -94.00  30.00   50
 27  \w     56.00 105.00   0.50   10.00    --   83.50-113.00-171.07   98
;
_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      0.0623938000
_diffrn_orient_matrix_UB_12      -0.0477648000
_diffrn_orient_matrix_UB_13      -0.0042713000
_diffrn_orient_matrix_UB_21      0.1072988000
_diffrn_orient_matrix_UB_22      0.0271741000
_diffrn_orient_matrix_UB_23      0.0128922000
_diffrn_orient_matrix_UB_31      -0.0115661000
_diffrn_orient_matrix_UB_32      -0.0064862000
_diffrn_orient_matrix_UB_33      0.0841045000
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            59316
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.724
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.533
_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    1.530
_exptl_crystal_description       needle
_exptl_crystal_F_000             2908
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         12529
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0699P)^2^+10.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9843
_reflns_number_total             12529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00490c2.cif
_cod_data_source_block           L2Y
_cod_original_cell_volume        6222.30(15)
_cod_database_code               7720828
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H51 N5 O7 F18 Y1 '
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.332
_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. Restrained distances
 C12B-C10B
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) = Uanis(C12B)
4. Others
 Sof(O1B)=Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=Sof(H31D)=
 Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O1A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=FVAR(1)
 Sof(H8BC)=Sof(H8BD)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10B)=
 Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=1-FVAR(2)
 Sof(H8AA)=Sof(H8AB)=Sof(C9A)=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(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(3)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C10A(H10A), C10B(H10B), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8AA,H8AB), C8(H8BC,H8BD), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C25(H25A,H25B),
 C26(H26A,H26B), C30A(H30A,H30B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,
 H33B), C30B(H30C,H30D), C31B(H31C,H31D), C32B(H32C,H32D), C33B(H33C,H33D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C16(H16), C20(H20), C21(H21), C22(H22),
 C23(H23), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C46(H46), C47(H47), C52(H52), C57(H57), C62(H62)
5.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              63573
_shelx_hkl_checksum              7387
_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.571