Field-assisted slow relaxation of magnetization in Cu(ii) complexes with pentaheterocyclic triphenodioxazine ligands: the quasi-one-dimensional versus the binuclear case
Korchagin, D. V.; Ivakhnenko, E. P.; Demidov, O. P.; Knyazev, P. A.; Efimov, N. N.; Morgunov, R. B.; Starikov, A. G.; Palii, A. V.; Minkin, V. I.; Aldoshin, S. M.; New Journal of Chemistry 47 (2023) 21353–21360; doi:10.1039/D3NJ04614A

data_7062847
_publ_section_title
;
 Field-assisted slow relaxation of magnetization in Cu(ii) complexes with
 pentaheterocyclic triphenodioxazine ligands: the quasi-one-dimensional
 versus the binuclear case
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21353
_journal_page_last               21360
_journal_paper_doi               10.1039/D3NJ04614A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C54 H46 Cu2 F24 N2 O10'
_chemical_formula_sum            'C54 H46 Cu2 F24 N2 O10'
_chemical_formula_weight         1466.01
_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
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.681(4)
_cell_angle_beta                 103.799(4)
_cell_angle_gamma                107.618(4)
_cell_formula_units_Z            1
_cell_length_a                   9.3736(5)
_cell_length_b                   13.0106(6)
_cell_length_c                   13.5156(7)
_cell_measurement_reflns_used    11307
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0110
_cell_measurement_theta_min      4.3020
_cell_volume                     1473.32(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_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    -65.00  33.00   1.00    1.00    --  -40.82  38.00-150.00   98
  2  \w   -129.00  47.00   1.00    1.00    --  -40.82   0.00   0.00  176
  3  \w      6.00  82.00   1.00    1.00    --   40.82 -99.00   0.00   76
  4  \w      7.00  42.00   1.00    1.00    --   40.82  82.00 -47.90   35
  5  \w      8.00  42.00   1.00    1.00    --   40.82  78.00-126.95   34
  6  \w      6.00  32.00   1.00    1.00    --   40.82  85.00 -86.06   26
  7  \w     27.00  97.00   1.00    1.00    --   40.82-125.00 120.00   70
  8  \w     84.00 178.00   1.00    3.03    --  112.00  30.00   0.00   94
  9  \w     84.00 178.00   1.00    3.03    --  112.00  30.00 -90.00   94
 10  \w     40.00 139.00   1.00    3.03    --  112.00 -52.00  57.88   99
 11  \w     39.00 138.00   1.00    3.03    --  112.00 -45.00-180.00   99
 12  \w     30.00 106.00   1.00    3.03    --  112.00 -95.00 150.00   76
 13  \w    103.00 178.00   1.00    3.03    --  112.00  77.00 150.00   75
 14  \w     30.00 106.00   1.00    3.03    --  112.00 -95.00 -60.00   76
 15  \w     30.00 106.00   1.00    3.03    --  112.00 -95.00  90.00   76
 16  \w    104.00 178.00   1.00    3.03    --  112.00 111.00-180.00   74
 17  \w     36.00 109.00   1.00    3.03    --  112.00-111.00  60.00   73
 18  \w     36.00 109.00   1.00    3.03    --  112.00-111.00-150.00   73
 19  \w     86.00 178.00   1.00    3.03    --  112.00  45.00-150.00   92
 20  \w     39.00 138.00   1.00    3.03    --  112.00 -45.00 -60.00   99
 21  \w    103.00 178.00   1.00    3.03    --  112.00  77.00-120.00   75
 22  \w     30.00 106.00   1.00    3.03    --  112.00 -95.00-120.00   76
 23  \w     84.00 178.00   1.00    3.03    --  112.00  30.00 120.00   94
 24  \w     83.00 178.00   1.00    3.03    --  112.00  61.00-180.00   95
 25  \w     30.00 106.00   1.00    3.03    --  112.00 -95.00 120.00   76
 26  \w     36.00 109.00   1.00    3.03    --  112.00-111.00 -60.00   73
 27  \w     36.00 109.00   1.00    3.03    --  112.00-111.00-120.00   73
 28  \w     39.00 138.00   1.00    3.03    --  112.00 -45.00-120.00   99
 29  \w     61.00 146.00   1.00    3.03    --  112.00 178.00-120.00   85
 30  \w     36.00 109.00   1.00    3.03    --  112.00-111.00   0.00   73
 31  \w     40.00 141.00   1.00    3.03    --  112.00 -61.00-180.00  101
 32  \w    104.00 178.00   1.00    3.03    --  112.00 111.00 120.00   74
 33  \w    103.00 178.00   1.00    3.03    --  112.00  77.00 120.00   75
 34  \w     61.00 146.00   1.00    3.03    --  112.00 178.00 150.00   85
 35  \w     83.00 136.00   1.00    3.03    --  112.00  61.00  60.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0062385000
_diffrn_orient_matrix_UB_12      0.0597972000
_diffrn_orient_matrix_UB_13      0.1103397000
_diffrn_orient_matrix_UB_21      0.1811399000
_diffrn_orient_matrix_UB_22      0.0449560000
_diffrn_orient_matrix_UB_23      0.0333257000
_diffrn_orient_matrix_UB_31      -0.0015935000
_diffrn_orient_matrix_UB_32      0.1046603000
_diffrn_orient_matrix_UB_33      -0.0385609000
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24302
_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         76.199
_diffrn_reflns_theta_min         3.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       prism
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0897P)^2^+0.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5381
_reflns_number_total             6115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04614a2.cif
_cod_data_source_block           ei_1502_autored
_cod_depositor_comments
'Adding full bibliography for 7062847--7062848.cif.'
_cod_database_code               7062847
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H46 Cu2 F24 N2 O10'
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1), C22(H22), C3(H3), C19(H19)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              37941
_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 2.366
_oxdiff_exptl_absorpt_empirical_full_min 0.510