Sterically crowded phenanthrolinediamides: conformational behavior and photophysics of their complexes with an Eu-Gd-Tb triad.
Avagyan, Nane A.; Zonov, Roman V.; Lemport, Pavel S.; Polikovskiy, Trofim A.; Metlin, Mikhail T.; Taydakov, Ilya V.; Averin, Alexei D.; Roznyatovsky, Vitaly A.; Simochkina, Anastasia I.; Danshina, Anastasia A.; Nelyubina, Yulia V.; Vokuev, Mikhail F.; Rodin, Igor A.; Ustynyuk, Yuri A.; Nenajdenko, Valentine G.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3055–3072; doi:10.1039/d5dt02745d

data_7720190
_publ_section_title
;
 Sterically crowded phenanthrolinediamides: conformational behavior and
 photophysics of their complexes with an Eu-Gd-Tb triad.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3055
_journal_page_last               3072
_journal_paper_doi               10.1039/d5dt02745d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C34 H34 N4 O2, 0.5(H2 O)'
_chemical_formula_sum            'C34 H35 N4 O2.5'
_chemical_formula_weight         539.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-09-23 deposited with the CCDC.	2026-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                87.6360(10)
_cell_angle_beta                 84.5140(10)
_cell_angle_gamma                65.9060(10)
_cell_formula_units_Z            4
_cell_length_a                   14.1554(2)
_cell_length_b                   14.3468(2)
_cell_length_c                   15.5469(2)
_cell_measurement_reflns_used    37796
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.3830
_cell_measurement_theta_min      2.8100
_cell_volume                     2869.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.44.118a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.114a 64-bit (release 13-06-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.118a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_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    -80.00  27.00   0.50    2.25    --  -44.25  98.00 -37.00  214
  2  \w     -5.00  81.00   0.50    2.25    --   44.25 -98.00-144.00  172
  3  \w     -5.00  81.00   0.50    2.25    --   44.25 -98.00-144.00  172
  4  \w   -170.00 -86.00   0.50    9.00    --  -96.00 -98.00-144.00  168
  5  \w    106.00 178.00   0.50    9.00    --  117.50  98.00 -37.00  144
  6  \w     45.00 106.00   0.50    9.00    --  117.50 -98.00-144.00  122
  7  \w    -43.00  32.00   0.50    2.25    --  -44.25  38.00 -30.00  150
  8  \w    -64.00  30.00   0.50    2.25    --  -44.25  57.00  90.00  188
  9  \w   -117.00 -17.00   0.50    2.25    --  -44.25 -77.00-180.00  200
 10  \w    -64.00  30.00   0.50    2.25    --  -44.25  57.00  90.00  188
 11  \w    -34.00  27.00   0.50    2.25    --   44.25 -19.00 -60.00  122
 12  \w    -34.00  27.00   0.50    2.25    --   44.25 -19.00-150.00  122
 13  \w     34.00  96.00   0.50    2.25    --   44.25-125.00-150.00  124
 14  \w   -170.00 -75.00   0.50    9.00    --  -96.00 -55.00 -80.14  190
 15  \w    -71.00 -22.00   0.50    9.00    --  -96.00  61.00   0.00   98
 16  \w    -51.00 -21.00   0.50    9.00    --  -96.00  45.00-120.00   60
 17  \w    -80.00 -22.00   0.50    9.00    --  -96.00  98.00 -37.00  116
 18  \w    -51.00 -21.00   0.50    9.00    --  -96.00  45.00 150.00   60
 19  \w     98.00 178.00   0.50    9.00    --  117.50  45.00 -60.00  160
 20  \w     45.00 111.00   0.50    9.00    --  117.50-125.00  60.00  132
 21  \w     98.00 178.00   0.50    9.00    --  117.50  45.00 -90.00  160
 22  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00 -30.00  120
 23  \w     98.00 178.00   0.50    9.00    --  117.50  45.00-120.00  160
 24  \w     97.00 178.00   0.50    9.00    --  117.50  61.00-120.00  162
 25  \w     45.00  71.00   0.50    9.00    --  117.50 -61.00 120.00   52
 26  \w     97.00 178.00   0.50    9.00    --  117.50  61.00-120.00  162
 27  \w     95.00 178.00   0.50    9.00    --  117.50 125.00 150.00  166
 28  \w     45.00 111.00   0.50    9.00    --  117.50-125.00  90.00  132
 29  \w     45.00  71.00   0.50    9.00    --  117.50 -61.00-180.00   52
 30  \w     91.00 178.00   0.50    9.00    --  117.50  77.00 120.00  174
 31  \w     91.00 178.00   0.50    9.00    --  117.50  77.00 120.00  174
 32  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00 -60.00  120
 33  \w     45.00 111.00   0.50    9.00    --  117.50-125.00-150.00  132
 34  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00 -90.00  120
 35  \w     45.00 111.00   0.50    9.00    --  117.50-125.00-120.00  132
 36  \w     45.00 111.00   0.50    9.00    --  117.50-125.00 150.00  132
 37  \w     45.00 111.00   0.50    9.00    --  117.50-125.00 120.00  132
 38  \w     91.00 178.00   0.50    9.00    --  117.50  77.00   0.00  174
 39  \w     45.00  71.00   0.50    9.00    --  117.50 -61.00 -60.00   52
 40  \w     86.00 178.00   0.50    9.00    --  117.50  15.00  90.00  184
 41  \w     91.00 178.00   0.50    9.00    --  117.50  77.00   0.00  174
 42  \w     45.00  71.00   0.50    9.00    --  117.50 -61.00 -30.00   52
 43  \w     86.00 178.00   0.50    9.00    --  117.50  15.00-180.00  184
 44  \w     45.00  71.00   0.50    9.00    --  117.50 -61.00 150.00   52
 45  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00-120.00  120
 46  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00 150.00  120
 47  \w     86.00 178.00   0.50    9.00    --  117.50  15.00-180.00  184
 48  \w     98.00 178.00   0.50    9.00    --  117.50  30.00 -30.00  160
 49  \w     45.00 111.00   0.50    9.00    --  117.50-125.00 150.00  132
 50  \w     95.00 178.00   0.50    9.00    --  117.50 125.00 150.00  166
 51  \w     45.00 111.00   0.50    9.00    --  117.50-125.00  30.00  132
 52  \w     45.00 111.00   0.50    9.00    --  117.50-125.00 -90.00  132
 53  \w     98.00 178.00   0.50    9.00    --  117.50  45.00 -60.00  160
 54  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00 120.00  120
 55  \w     98.00 178.00   0.50    9.00    --  117.50  45.00  30.00  160
 56  \w     98.00 178.00   0.50    9.00    --  117.50  30.00 120.00  160
 57  \w     98.00 178.00   0.50    9.00    --  117.50  30.00 120.00  160
 58  \w     45.00 105.00   0.50    9.00    --  117.50 -77.00  60.00  120
 59  \w     45.00 105.00   0.50    9.00    --  117.50 -95.00  60.00  120
 60  \w     45.00 111.00   0.50    9.00    --  117.50-125.00   0.00  132
 61  \w     45.00 111.00   0.50    9.00    --  117.50-125.00 120.00  132
 62  \w   -117.00 -17.00   0.50    2.25    --  -44.25 -77.00   0.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65818
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         2.855
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.118a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.249
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         10315
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0699P)^2^+1.7886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8937
_reflns_number_total             10315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02745d3.cif
_cod_data_source_block           l2
_cod_original_formula_sum        'C34 H35 N4 O2.50'
_cod_database_code               7720190
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C34H35N4O2.5
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.934
_diffrn_oxdiff_digest_hkl
;
439aea82dc302fb0dbc3667e31d2da9e9fcbe7
;
_diffrn_oxdiff_measurement_exp_name 25DAA_R072.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-C44 \\sim C23A-C20A
 with sigma of 0.02
 C22A-C17A \\sim C43-C38
 with sigma of 0.02
 C23A-C20A \\sim C44-C41
 with sigma of 0.02
 N3A-C16A \\sim N3A"-C16A
 with sigma of 0.02
 N3A-C13A \\sim N3A"-C13A
 with sigma of 0.02
 N3A"-C35 \\sim N3A-C14A
 with sigma of 0.02
 N3A"-C37 \\sim N3A-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C18A)
\\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C16A) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C23A) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N3A") \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C36) = Uanis(C15A)
Uanis(C35) = Uanis(C14A)
Uanis(N3A") = Uanis(N3A)
Uanis(C38) = Uanis(C21A)
Uanis(C17A) = Uanis(C42)
Uanis(C16A) = Uanis(C37)
Uanis(C41) = Uanis(C18A)
Uanis(C20A) = Uanis(C39)
Uanis(C40) = Uanis(C19A)
Uanis(C23A) = Uanis(C44)
Uanis(C44) = Uanis(C23A)
Uanis(C43) = Uanis(C22A)
4. Others
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=
 Sof(C42)=Sof(H42)=Sof(C41)=Sof(C40)=Sof(H40)=Sof(C39)=Sof(H39)=Sof(C38)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(N3A")=1-FVAR(1)
 Sof(N3A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C14A(H14A,H14B), C25A(H25A,H25B), C14(H14C,H14D), C25(H25C,
 H25D)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C40(H40), C39(H39), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A),
 C8A(H8A), C9A(H9A), C18A(H18A), C19A(H19A), C21A(H21A), C29A(H29A), C30A(H30A),
  C32A(H32A), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C18(H18),
 C19(H19), C21(H21), C29(H29), C30(H30), C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C37(C42,C41,C40,C39,C38), C16A(C17A,C18A,C19A,C20A,C21A)
5.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C15A(H15A,H15B,
 H15C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C26A(H26A,H26B,H26C),
 C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C15(H15D,H15E,H15F), C22(H22D,H22E,
 H22F), C23(H23D,H23E,H23F), C26(H26D,H26E,H26F), C33(H33D,H33E,H33F), C34(H34D,
 H34E,H34F)
;
_shelx_res_checksum              4978
_shelx_hkl_checksum              18789
_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 1.533
_oxdiff_exptl_absorpt_empirical_full_min 0.833