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

data_7720827
_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         'C49 H49 N5 O'
_chemical_formula_sum            'C49 H49 N5 O'
_chemical_formula_weight         723.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-08-12
_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                 94.1684(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.71021(19)
_cell_length_b                   17.83878(16)
_cell_length_c                   22.5695(2)
_cell_measurement_reflns_used    27094
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.7610
_cell_measurement_theta_min      2.8840
_cell_volume                     7914.58(13)
_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(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 0.987
_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 -24.00   0.50    3.00    --  -57.24 -15.00 -90.00  132
  2  \w    -86.00 -38.00   0.50    3.00    --  -57.24 125.00-180.00   96
  3  \w    -90.00 -30.00   0.50    3.00    --  -57.24 -15.00-150.00  120
  4  \w    -73.00 -35.00   0.50    3.00    --  -57.24 125.00   0.00   76
  5  \w     38.00  65.00   0.50    3.00    --   60.05 -94.00 -30.00   54
  6  \w     75.00 107.00   0.50    3.00    --   60.05  15.00 120.00   64
  7  \w     20.00  45.00   0.50    3.00    --   60.05 -94.00  30.00   50
  8  \w     35.00  74.00   0.50    3.00    --   60.05-125.00 -60.00   78
  9  \w     35.00  68.00   0.50    3.00    --   60.05 -94.00 120.00   66
 10  \w     48.00 100.00   0.50    3.00    --   60.05  15.00 -90.00  104
 11  \w     31.00  62.00   0.50    3.00    --   60.05  15.00 120.00   62
 12  \w     49.00  84.00   0.50    3.00    --   74.47 -94.00-120.00   70
 13  \w     40.00  65.00   0.50    3.00    --   79.86 -94.00-150.00   50
 14  \w     47.00  76.00   0.50    3.00    --   79.86  15.00-120.00   58
 15  \w     41.00  81.00   0.50    3.00    --   79.86-125.00 120.00   80
 16  \w     46.00  80.00   0.50    3.00    --   79.86-125.00 150.00   68
 17  \w     41.00  85.00   0.50    3.00    --   79.86 -94.00 -30.00   88
 18  \w     47.00 126.00   0.50    3.00    --   79.86  15.00 -90.00  158
 19  \w     55.00  88.00   0.50    3.00    --   79.86 -94.00 -60.00   66
 20  \w     50.00 109.00   0.50    3.00    --   79.86  15.00   0.00  118
 21  \w     40.00  65.00   0.50    3.00    --   79.86 -94.00  60.00   50
 22  \w     40.00  89.00   0.50    3.00    --   79.86 -94.00 150.00   98
 23  \w     58.00  88.00   0.50    3.00    --   79.86 -94.00  30.00   60
 24  \w     45.00  88.00   0.50    3.00    --   79.86 -94.00   0.00   86
 25  \w     47.00  79.00   0.50    3.00    --   79.86  15.00-180.00   64
 26  \w     90.00 115.00   0.50    3.00    --   79.86  15.00-180.00   50
 27  \w     40.00  87.00   0.50    3.00    --   79.86 -94.00-180.00   94
 28  \w     79.00 104.00   0.50    3.00    --   79.86  15.00-120.00   50
 29  \w     55.00 118.00   0.50    3.00    --   79.86  15.00  90.00  126
;
_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      -0.0032260000
_diffrn_orient_matrix_UB_12      -0.0564315000
_diffrn_orient_matrix_UB_13      0.0513341000
_diffrn_orient_matrix_UB_21      0.0754035000
_diffrn_orient_matrix_UB_22      -0.0198226000
_diffrn_orient_matrix_UB_23      -0.0051663000
_diffrn_orient_matrix_UB_31      0.0210069000
_diffrn_orient_matrix_UB_32      0.0623356000
_diffrn_orient_matrix_UB_33      0.0449673000
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76881
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.289
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.911
_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    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         15921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0772P)^2^+1.8860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12857
_reflns_number_total             15921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00490c2.cif
_cod_data_source_block           L2
_cod_database_code               7720827
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C49 H49 N5 O1 '
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.890
_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:
 C10(H10), C27(H27), C10B(H10B), C27B(H27B)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C25(H25A,H25B), C26(H26A,H26B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C8B(H8BA,H8BB), C9B(H9BA,H9BB),
  C25B(H25C,H25D), C26B(H26C,H26D), C30B(H30C,H30D), C31B(H31C,H31D), C32B(H32C,
 H32D), C33B(H33C,H33D)
2.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), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B),
 C14B(H14B), C16B(H16B), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B),
 C35B(H35B), C36B(H36B), C38B(H38B), C39B(H39B), C41B(H41B), C42B(H42B),
 C43B(H43B), C45B(H45B), C46B(H46B)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C28B(H28D,H28E,H28F),
 C29B(H29D,H29E,H29F)
;
_shelx_res_checksum              86709
_shelx_hkl_checksum              11307
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.698