Synthesis, Structural and Photophysical Studies of Mono-and Dinuclear Alkali Metal 2,6-dibenzhydryl-4-methylphenolates
Bardonov, Daniil; Nasyrova, Darina; Metlin, Mikhail T.; Minyaev, Mikhail E.; Taydakov, Ilya V.; Roitershtein, Dmitrii M.; New Journal of Chemistry  (2026) –; doi:10.1039/D5NJ03734D

data_7064166
_publ_section_title
;
 Synthesis, Structural and Photophysical Studies of Mono-and Dinuclear
 Alkali Metal 2,6-dibenzhydryl-4-methylphenolates
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D5NJ03734D
_journal_year                    2026
_chemical_formula_moiety         'C45 H51 Na O7'
_chemical_formula_sum            'C45 H51 Na O7'
_chemical_formula_weight         726.84
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2025-12-02 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                80.8380(10)
_cell_angle_beta                 68.5020(10)
_cell_angle_gamma                72.6630(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0879(2)
_cell_length_b                   13.4341(2)
_cell_length_c                   14.7219(2)
_cell_measurement_reflns_used    41349
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      77.5250
_cell_measurement_theta_min      3.2140
_cell_volume                     1944.57(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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    -52.00  24.00   0.50    0.30    --  -48.70  46.00 -57.00  152
  2  \w   -120.00 -37.00   0.50    0.30    --  -48.70 -46.00 153.00  166
  3  \w    -22.00  52.00   0.50    0.30    --   48.70 -46.00 153.00  148
  4  \w   -158.00 -75.00   0.50    0.85    --  -86.25 -46.00 153.00  166
  5  \w    -52.00 -14.00   0.50    0.85    --  -86.25  46.00 -57.00   76
  6  \w     97.00 178.00   0.50    0.85    --  107.75  46.00 -57.00  162
  7  \w   -118.00 -73.00   0.50    0.30    --  -48.70-125.00  90.00   90
  8  \w   -118.00 -73.00   0.50    0.30    --  -48.70-125.00 -60.00   90
  9  \w     34.00  93.00   0.50    0.30    --   48.70-125.00   0.00  118
 10  \w    -23.00  43.00   0.50    0.30    --   48.70 -38.00 -90.00  132
 11  \w     34.00  93.00   0.50    0.30    --   48.70-125.00  90.00  118
 12  \w    -25.00  26.00   0.50    0.30    --   48.70 -19.00   0.00  102
 13  \w     38.00 120.00   0.50    0.30    --   48.70  46.00 -57.00  164
 14  \w    -71.00 -14.00   0.50    0.85    --  -86.25  61.00 -60.00  114
 15  \w     89.00 178.00   0.50    0.85    --  107.75  70.00 168.98  178
 16  \w     36.00  71.00   0.50    0.85    --  107.75 -61.00 -30.00   70
 17  \w     36.00 105.00   0.50    0.85    --  107.75 -77.00 120.00  138
 18  \w     97.00 178.00   0.50    0.85    --  107.75  30.00 -90.00  162
 19  \w     39.00 111.00   0.50    0.85    --  107.75-125.00-180.00  144
 20  \w     39.00 111.00   0.50    0.85    --  107.75-125.00  30.00  144
 21  \w     97.00 168.00   0.50    0.85    --  107.75  45.00-150.00  142
 22  \w     77.00 105.00   0.50    0.85    --  107.75-102.00-132.74   56
 23  \w    105.00 134.00   0.50    0.85    --  107.75 125.00  30.00   58
 24  \w     39.00  66.00   0.50    0.85    --  107.75-102.00-132.74   54
 25  \w     81.00 106.00   0.50    0.85    --  107.75-106.00-100.65   50
 26  \w    145.00 171.00   0.50    0.85    --  107.75 125.00  30.00   52
 27  \w     43.00  73.00   0.50    0.85    --  107.75 -95.00  30.00   60
 28  \w     78.00 103.00   0.50    0.85    --  107.75 -95.00  30.00   50
 29  \w     93.00 124.00   0.50    0.85    --  107.75 -87.00  47.92   62
 30  \w     63.00 111.00   0.50    0.85    --  107.75-125.00   0.00   96
 31  \w     36.00  71.00   0.50    0.85    --  107.75 -61.00-150.00   70
 32  \w    121.00 147.00   0.50    0.85    --  107.75  30.00  60.00   52
 33  \w    124.00 150.00   0.50    0.85    --  107.75  45.00 -60.00   52
 34  \w     36.00  70.00   0.50    0.85    --  107.75 -61.00  90.00   68
 35  \w     39.00  81.00   0.50    0.85    --  107.75 -95.00 -90.00   84
 36  \w     37.00  70.00   0.50    0.85    --  107.75 -61.00 -90.00   66
 37  \w     92.00 120.00   0.50    0.85    --  107.75-136.00-118.32   56
 38  \w    103.00 129.00   0.50    0.85    --  107.75  45.00  90.00   52
 39  \w     62.00  99.00   0.50    0.85    --  107.75-123.00-146.88   74
 40  \w     36.00  71.00   0.50    0.85    --  107.75 -61.00  30.00   70
 41  \w    104.00 178.00   0.50    0.85    --  107.75  77.00-150.00  148
 42  \w     93.00 151.00   0.50    0.85    --  107.75  61.00  -8.78  116
 43  \w     97.00 178.00   0.50    0.85    --  107.75  15.00 150.00  162
 44  \w     36.00  61.00   0.50    0.85    --  107.75 -95.00-150.00   50
 45  \w     67.00  93.00   0.50    0.85    --  107.75 -95.00-150.00   52
 46  \w     36.00  91.00   0.50    0.85    --  107.75 -83.00 -14.66  110
 47  \w    107.00 132.00   0.50    0.85    --  107.75 -83.00 -14.66   50
 48  \w    104.00 161.00   0.50    0.85    --  107.75  45.00  30.00  114
 49  \w     39.00  66.00   0.50    0.85    --  107.75 -61.00 120.00   54
 50  \w     39.00 110.00   0.50    0.85    --  107.75-125.00 -60.00  142
 51  \w     65.00 111.00   0.50    0.85    --  107.75-125.00 -30.00   92
 52  \w     36.00  67.00   0.50    0.85    --  107.75 -87.00  47.92   62
 53  \w     73.00 104.00   0.50    0.85    --  107.75 -77.00  30.00   62
 54  \w     43.00  69.00   0.50    0.85    --  107.75 -95.00  90.00   52
 55  \w     38.00  72.00   0.50    0.85    --  107.75-129.00-115.61   68
 56  \w     86.00 115.00   0.50    0.85    --  107.75-129.00-115.61   58
 57  \w     99.00 134.00   0.50    0.85    --  107.75 125.00 -60.00   70
 58  \w    142.00 168.00   0.50    0.85    --  107.75 125.00 -60.00   52
 59  \w    120.00 163.00   0.50    0.85    --  107.75 125.00  90.00   86
 60  \w     40.00  67.00   0.50    0.85    --  107.75 -77.00-150.00   54
 61  \w     70.00  96.00   0.50    0.85    --  107.75 -95.00 -60.00   52
 62  \w     38.00  84.00   0.50    0.85    --  107.75 -77.00  60.00   92
 63  \w     92.00 174.00   0.50    0.85    --  107.75  77.00-120.00  164
 64  \w     66.00 109.00   0.50    0.85    --  107.75 -80.00 -61.43   86
 65  \w     66.00  92.00   0.50    0.85    --  107.75 -77.00   0.00   52
 66  \w     40.00  66.00   0.50    0.85    --  107.75 -74.00-137.36   52
 67  \w     52.00  85.00   0.50    0.85    --  107.75   0.00-180.00   66
 68  \w     66.00 106.00   0.50    0.85    --  107.75-108.00 132.18   80
 69  \w     62.00  88.00   0.50    0.85    --  107.75-131.00 146.91   52
 70  \w     80.00 111.00   0.50    0.85    --  107.75-125.00 150.00   62
 71  \w     37.00  70.00   0.50    0.85    --  107.75 -95.00 -30.00   66
 72  \w     74.00 104.00   0.50    0.85    --  107.75 -95.00 -30.00   60
 73  \w     78.00 104.00   0.50    0.85    --  107.75 -95.00 150.00   52
 74  \w     78.00 110.00   0.50    0.85    --  107.75-125.00 -90.00   64
 75  \w     68.00 102.00   0.50    0.85    --  107.75-125.00  60.00   68
 76  \w     42.00  68.00   0.50    0.85    --  107.75-106.00-100.65   52
 77  \w     97.00 177.00   0.50    0.85    --  107.75  30.00-180.00  160
 78  \w    103.00 173.00   0.50    0.85    --  107.75  30.00 -60.00  140
 79  \w    126.00 152.00   0.50    0.85    --  107.75  30.00 150.00   52
 80  \w    129.00 158.00   0.50    0.85    --  107.75  15.00 120.00   58
 81  \w    100.00 126.00   0.50    0.85    --  107.75  61.00 -90.00   52
 82  \w     94.00 120.00   0.50    0.85    --  107.75  61.00 -30.00   52
 83  \w     86.00 120.00   0.50    0.85    --  107.75  77.00 150.00   68
 84  \w    139.00 164.00   0.50    0.85    --  107.75  77.00 150.00   50
 85  \w     64.00  90.00   0.50    0.85    --  107.75 -81.00 146.90   52
 86  \w     73.00 107.00   0.50    0.85    --  107.75-100.00  27.08   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0795940000
_diffrn_orient_matrix_UB_12      -0.0444569000
_diffrn_orient_matrix_UB_13      -0.0427739000
_diffrn_orient_matrix_UB_21      -0.0463207000
_diffrn_orient_matrix_UB_22      0.1084729000
_diffrn_orient_matrix_UB_23      -0.0477237000
_diffrn_orient_matrix_UB_31      0.1242872000
_diffrn_orient_matrix_UB_32      -0.0271138000
_diffrn_orient_matrix_UB_33      -0.0926405000
_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     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51310
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.855
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
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_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.00162(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0366P)^2^+0.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7885
_reflns_number_total             8226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03734d2.cif
_cod_data_source_block           naoarcrown
_cod_database_code               7064166
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H10O3Na
_chemical_oxdiff_usercomment     NaOArCrown
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.723
_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:
 C7(H7), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              31348
_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 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.698