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

data_7720824
_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         'C67 H61 N5'
_chemical_formula_sum            'C67 H61 N5'
_chemical_formula_weight         936.20
_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             2025-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7205)
;
_audit_update_record
;
2026-02-17 deposited with the CCDC.	2026-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8568(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0953(2)
_cell_length_b                   12.63448(11)
_cell_length_c                   16.11327(12)
_cell_measurement_reflns_used    25945
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      74.0730
_cell_measurement_theta_min      2.8080
_cell_volume                     5157.94(7)
_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    -86.00 -36.00   0.50    1.50    --  -57.24 125.00  90.00  100
  2  \w    -70.00 -36.00   0.50    1.50    --  -57.24 125.00 -30.00   68
  3  \w    -85.00 -36.00   0.50    1.50    --  -57.24 125.00  30.00   98
  4  \w    -85.00 -59.00   0.50    1.50    --  -57.24 125.00-120.00   52
  5  \w     28.00  55.00   0.50    1.50    --   60.05  15.00  30.00   54
  6  \w     36.00  62.00   0.50    1.50    --   60.05-125.00-120.00   52
  7  \w     27.00  66.00   0.50    1.50    --   60.05  15.00-180.00   78
  8  \w     68.00 106.00   0.50    1.50    --   60.05  15.00  30.00   76
  9  \w     75.00 107.00   0.50    1.50    --   60.05  15.00-180.00   64
 10  \w     35.00  89.00   0.50    1.50    --   60.05-125.00 -60.00  108
 11  \w     44.00  70.00   0.50    1.50    --   60.05-125.00   0.00   52
 12  \w     20.00  45.00   0.50    1.50    --   60.05 -94.00 -30.00   50
 13  \w     35.00  72.00   0.50    1.50    --   60.05-125.00 120.00   74
 14  \w     48.00  76.00   0.50    1.50    --   74.47 -94.00   0.00   56
 15  \w     40.00  83.00   0.50    1.50    --   79.86 -94.00  90.00   86
 16  \w     52.00  78.00   0.50    1.50    --   79.86  15.00  60.00   52
 17  \w     43.00  79.00   0.50    1.50    --   79.86 -94.00 120.00   72
 18  \w     41.00  75.00   0.50    1.50    --   79.86 -94.00 -90.00   68
 19  \w    101.00 126.00   0.50    1.50    --   79.86  15.00 150.00   50
 20  \w     49.00  74.00   0.50    1.50    --   79.86 -94.00 -30.00   50
 21  \w     36.00  90.00   0.50    1.50    --   79.86-125.00  30.00  108
 22  \w     52.00  87.00   0.50    1.50    --   79.86 -94.00 150.00   70
 23  \w     43.00  82.00   0.50    1.50    --   79.86 -94.00  30.00   78
 24  \w     48.00  83.00   0.50    1.50    --   79.86  15.00-120.00   70
 25  \w     41.00  69.00   0.50    1.50    --   79.86 -94.00-180.00   56
 26  \w     42.00  90.00   0.50    1.50    --   79.86 -94.00 -60.00   96
 27  \w     50.00 125.00   0.50    1.50    --   79.86  15.00   0.00  150
 28  \w    101.00 126.00   0.50    1.50    --   79.86  15.00  60.00   50
 29  \w     43.00  79.00   0.50    1.50    --   79.86 -94.00-150.00   72
 30  \w     54.00  79.00   0.50    1.50    --   79.86-125.00-150.00   50
 31  \w     38.00  64.00   0.50    1.50    --   79.86-118.00 124.00   52
 32  \w     48.00  93.00   0.50    1.50    --   79.86  15.00 -60.00   90
 33  \w     40.00  89.00   0.50    1.50    --   79.86 -94.00  60.00   98
 34  \w     83.00 108.00   0.50    1.50    --   79.86-125.00-120.00   50
 35  \w     57.00  96.00   0.50    1.50    --   79.86  15.00 150.00   78
;
_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      0.0588435000
_diffrn_orient_matrix_UB_12      0.0305375000
_diffrn_orient_matrix_UB_13      0.0209551000
_diffrn_orient_matrix_UB_21      -0.0128832000
_diffrn_orient_matrix_UB_22      0.1042222000
_diffrn_orient_matrix_UB_23      0.0403062000
_diffrn_orient_matrix_UB_31      0.0082537000
_diffrn_orient_matrix_UB_32      -0.0554348000
_diffrn_orient_matrix_UB_33      0.0873837000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53092
_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         74.250
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.877
_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    1.206
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0594P)^2^+2.2540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9124
_reflns_number_total             10382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00490c2.cif
_cod_data_source_block           L1
_cod_original_cell_volume        5157.94(8)
_cod_database_code               7720824
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C67 H61 N5 '
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.830
_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), C46(H46)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C44(H44A,H44B), C45(H45A,H45B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C39(H39),
  C41(H41), C42(H42), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59),
 C60(H60), C61(H61), C63(H63), C64(H64)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              44624
_shelx_hkl_checksum              46240
_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 1.570
_oxdiff_exptl_absorpt_empirical_full_min 0.584