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

data_7720829
_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         'C82 H64 F18 N5 O6 Y, 2.25[C6H14]'
_chemical_formula_sum            'C95.5 H95.5 F18 N5 O6 Y'
_chemical_formula_weight         1840.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2026-02-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.11679(14)
_cell_length_b                   14.05917(8)
_cell_length_c                   30.12016(14)
_cell_measurement_reflns_used    31871
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      75.1250
_cell_measurement_theta_min      2.9290
_cell_volume                     8518.75(9)
_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 0.975
_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    -63.00 -23.00   0.50    2.00    --  -57.24 -12.00 -52.00   80
  2  \w    -86.00 -35.00   0.50    2.00    --  -57.24 125.00 150.00  102
  3  \w   -104.00 -69.00   0.50    2.00    --  -57.24 -12.00 -52.00   70
  4  \w    -69.00 -35.00   0.50    2.00    --  -57.24 125.00 -90.00   68
  5  \w   -104.00 -35.00   0.50    2.00    --  -57.24 -15.00-150.00  138
  6  \w     22.00  52.00   0.50    2.00    --   60.05 -94.00 120.00   60
  7  \w     51.00  86.00   0.50    2.00    --   60.05-157.00  53.00   70
  8  \w     35.00  85.00   0.50    2.00    --   60.05-125.00 -60.00  100
  9  \w     40.00  87.00   0.50    2.00    --   60.05-125.00-180.00   94
 10  \w     68.00  96.00   0.50    2.00    --   74.47-125.00 -90.00   56
 11  \w     88.00 113.00   0.50    2.00    --   74.47  15.00 150.00   50
 12  \w     38.00  63.00   0.50    2.00    --   74.47-125.00 -90.00   50
 13  \w     49.00  88.00   0.50    2.00    --   79.86 -94.00 -60.00   78
 14  \w     74.00 109.00   0.50    2.00    --   79.86-125.00 -90.00   70
 15  \w     50.00  85.00   0.50    2.00    --   79.86 -94.00  60.00   70
 16  \w     43.00  69.00   0.50    2.00    --   79.86-125.00-180.00   52
 17  \w     40.00  65.00   0.50    2.00    --   79.86 -94.00   0.00   50
 18  \w     43.00  85.00   0.50    2.00    --   79.86 -94.00  30.00   84
 19  \w     44.00  77.00   0.50    2.00    --   79.86 -94.00 120.00   66
 20  \w     77.00 105.00   0.50    2.00    --   79.86-119.00-151.00   56
 21  \w     54.00  86.00   0.50    2.00    --   79.86 -94.00 -30.00   64
 22  \w     55.00 104.00   0.50    2.00    --   79.86-125.00 -60.00   98
 23  \w     41.00  75.00   0.50    2.00    --   79.86 -94.00-150.00   68
 24  \w     47.00 107.00   0.50    2.00    --   79.86  12.00 119.00  120
 25  \w     63.00 108.00   0.50    2.00    --   79.86  15.00 -30.00   90
 26  \w     47.00 124.00   0.50    2.00    --   79.86  15.00 -90.00  154
 27  \w     49.00 132.00   0.50    2.00    --   83.50  18.00  28.34  166
;
_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      0.0720321000
_diffrn_orient_matrix_UB_12      0.0340679000
_diffrn_orient_matrix_UB_13      -0.0070097000
_diffrn_orient_matrix_UB_21      -0.0248255000
_diffrn_orient_matrix_UB_22      0.1031786000
_diffrn_orient_matrix_UB_23      -0.0045953000
_diffrn_orient_matrix_UB_31      0.0077246000
_diffrn_orient_matrix_UB_32      0.0140994000
_diffrn_orient_matrix_UB_33      0.0504600000
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.964
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.697
_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    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             3810
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1070P)^2^+9.9952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7394
_reflns_number_total             8673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00490c2.cif
_cod_data_source_block           L1Y
_cod_original_cell_volume        8518.75(8)
_cod_original_formula_sum        'C95.50 H95.50 F18 N5 O6 Y'
_cod_database_code               7720829
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C97 H82.50 N5 O6 F18 Y1 '
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C8(H8), C9(H9), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C42(H42)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 440 electrons were 
found in a volume of 1900\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.25[C6H14] per Unit Cell 
which account for 450 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37617
_shelx_hkl_checksum              38698
_shelx_fab_checksum              7650
_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.670