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_7064164
_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         'C74 H70 K2 O4'
_chemical_formula_sum            'C74 H70 K2 O4'
_chemical_formula_weight         1101.50
_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     direct
_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
;
2025-12-01 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.22670(10)
_cell_length_b                   14.83450(10)
_cell_length_c                   17.17330(10)
_cell_measurement_reflns_used    28594
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      77.5450
_cell_measurement_theta_min      3.7640
_cell_volume                     2989.08(4)
_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      99.97(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -81.00 -16.50   0.50    1.00    --  -86.25 101.00  40.00  129
  2  \w    -81.00  18.50   0.50    0.40    --  -48.70 101.00  40.00  199
  3  \w    -39.00  23.50   0.50    0.40    --  -48.70  38.00 -60.00  125
  4  \w    -14.00  14.00   0.50    0.40    --  -48.70  19.00-120.00   56
  5  \w    -43.00  19.50   0.50    0.40    --  -48.70  38.00-180.00  125
  6  \w     61.00 111.00   0.50    1.00    --  107.75-125.00-120.00  100
  7  \w     68.00 111.50   0.50    1.00    --  107.75-125.00 -30.00   87
  8  \w     40.00 106.00   0.50    1.00    --  107.75-104.00   3.72  132
  9  \w     52.00  84.00   0.50    1.00    --  107.75-125.00  60.00   64
 10  \w     78.00 106.00   0.50    1.00    --  107.75-108.00  24.77   56
 11  \w     76.00 106.50   0.50    1.00    --  107.75-114.00  12.21   61
 12  \w     47.00  73.50   0.50    1.00    --  107.75-101.00 -64.00   53
 13  \w     66.00  92.50   0.50    1.00    --  107.75 -95.00 -30.00   53
 14  \w      4.00  81.50   0.50    0.40    --   48.70-101.00 -64.00  155
 15  \w     36.00  66.50   0.50    1.00    --  107.75 -95.00  60.00   61
 16  \w     36.00  72.00   0.50    1.00    --  107.75 -95.00  90.00   72
 17  \w     45.00  83.00   0.50    1.00    --  107.75 -85.00 177.72   76
 18  \w     41.00  81.50   0.50    1.00    --  107.75 -98.00  89.01   81
 19  \w     78.00 104.50   0.50    1.00    --  107.75 -95.00  90.00   53
 20  \w     78.00 104.50   0.50    1.00    --  107.75 -95.00  60.00   53
 21  \w     73.00 123.50   0.50    1.00    --  107.75 -85.00  91.39  101
 22  \w     96.00 126.00   0.50    1.00    --  107.75 -85.00 177.72   60
 23  \w     45.00  71.50   0.50    1.00    --  107.75 -89.00  -2.08   53
 24  \w     84.00 110.50   0.50    1.00    --  107.75 -83.00 -94.59   53
 25  \w     51.00  83.00   0.50    1.00    --  107.75 -83.00 -94.59   64
 26  \w     36.00  78.00   0.50    1.00    --  107.75 -77.00-120.00   84
 27  \w     36.00  70.00   0.50    1.00    --  107.75 -61.00-150.00   68
 28  \w     38.00  72.50   0.50    1.00    --  107.75 -77.00 -60.00   69
 29  \w     44.00  69.50   0.50    1.00    --  107.75 -77.00   0.00   51
 30  \w     70.00  98.50   0.50    1.00    --  107.75 -77.00   0.00   57
 31  \w     37.00  71.00   0.50    1.00    --  107.75 -61.00 120.00   68
 32  \w    126.00 162.00   0.50    1.00    --  107.75  15.00 -30.00   72
 33  \w    125.00 175.50   0.50    1.00    --  107.75  77.00  30.00  101
 34  \w     97.00 123.50   0.50    1.00    --  107.75  77.00  30.00   53
 35  \w    102.00 127.50   0.50    1.00    --  107.75  45.00 -30.00   51
 36  \w    103.00 135.50   0.50    1.00    --  107.75  45.00-150.00   65
 37  \w    143.00 177.00   0.50    1.00    --  107.75  45.00-150.00   68
 38  \w    145.00 175.50   0.50    1.00    --  107.75  77.00-180.00   61
 39  \w    100.00 174.50   0.50    1.00    --  107.75  45.00-180.00  149
 40  \w     86.00 122.00   0.50    1.00    --  107.75  77.00-180.00   72
 41  \w    115.00 163.00   0.50    1.00    --  107.75  30.00 -90.00   96
 42  \w    141.00 166.50   0.50    1.00    --  107.75  45.00 -30.00   51
 43  \w    105.00 131.50   0.50    1.00    --  107.75  45.00   0.00   53
 44  \w    100.00 136.00   0.50    1.00    --  107.75  30.00  30.00   72
 45  \w    100.00 156.00   0.50    1.00    --  107.75  30.00 120.00  112
 46  \w    140.00 166.50   0.50    1.00    --  107.75 125.00  90.00   53
 47  \w     97.00 131.50   0.50    1.00    --  107.75 125.00 150.00   69
 48  \w    110.00 140.50   0.50    1.00    --  107.75 101.00  40.00   61
 49  \w    107.00 161.00   0.50    1.00    --  107.75  98.00-109.32  108
 50  \w   -145.00-119.50   0.50    1.00    --  -86.25-101.00 -64.00   51
 51  \w   -117.00 -74.50   0.50    0.40    --  -48.70-125.00  90.00   85
;
_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      0.0476338000
_diffrn_orient_matrix_UB_12      0.0967144000
_diffrn_orient_matrix_UB_13      0.0080463000
_diffrn_orient_matrix_UB_21      0.0715037000
_diffrn_orient_matrix_UB_22      -0.0206354000
_diffrn_orient_matrix_UB_23      0.0874304000
_diffrn_orient_matrix_UB_31      0.0992889000
_diffrn_orient_matrix_UB_32      -0.0317768000
_diffrn_orient_matrix_UB_33      -0.0320442000
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40549
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.868
_diffrn_reflns_theta_min         3.767
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.436
_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    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.3177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6169
_reflns_number_total             6373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03734d2.cif
_cod_data_source_block           koar
_cod_original_cell_volume        2989.07(4)
_cod_database_code               7064164
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20O2K
_chemical_oxdiff_usercomment     KOAr
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.634
_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), C18(H18), C19(H19), C21(H21), C26(H26), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
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), C23(H23), C24(H24), C25(H25), 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              36296
_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 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.753