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_7062848
_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         'C36 H28 Cu F12 N2 O6'
_chemical_formula_sum            'C36 H28 Cu F12 N2 O6'
_chemical_formula_weight         876.14
_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             2021-04-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                91.565(2)
_cell_angle_beta                 97.827(2)
_cell_angle_gamma                106.988(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5270(2)
_cell_length_b                   13.6628(3)
_cell_length_c                   15.3279(2)
_cell_measurement_reflns_used    16624
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.1090
_cell_measurement_theta_min      4.2990
_cell_volume                     1885.58(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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   -114.00 -14.00   1.00    4.25    --  -41.72 -57.00-150.00  100
  2  \w   -116.00 -17.00   1.00    4.25    --  -41.72 -38.00 -30.00   99
  3  \w    -66.00  33.00   1.00    4.25    --  -41.72  38.00 150.00   99
  4  \w      7.00  33.00   1.00    4.25    --   41.72  84.00 -37.33   26
  5  \w    -30.00  70.00   1.00    4.25    --   41.72 -57.00 -60.00  100
  6  \w     27.00  98.00   1.00    4.25    --   41.72-125.00-180.00   71
  7  \w     36.00 109.00   1.00   17.01    --  112.00-111.00-120.00   73
  8  \w    103.00 178.00   1.00   17.01    --  112.00  77.00-120.00   75
  9  \w     36.00 145.00   1.00   17.01    --  112.00 -77.00  60.00  109
 10  \w     36.00 109.00   1.00   17.01    --  112.00-111.00-180.00   73
 11  \w     39.00 138.00   1.00   17.01    --  112.00 -45.00  90.00   99
 12  \w     36.00 109.00   1.00   17.01    --  112.00-111.00   0.00   73
 13  \w     36.00 109.00   1.00   17.01    --  112.00-111.00 -90.00   73
 14  \w     36.00 109.00   1.00   17.01    --  112.00-111.00  30.00   73
 15  \w    104.00 178.00   1.00   17.01    --  112.00 111.00-120.00   74
 16  \w     36.00 140.00   1.00   17.01    --  112.00 -30.00-180.00  104
 17  \w     30.00 106.00   1.00   17.01    --  112.00 -95.00  90.00   76
 18  \w     86.00 178.00   1.00   17.01    --  112.00  45.00  30.00   92
 19  \w     36.00 109.00   1.00   17.01    --  112.00-111.00-150.00   73
 20  \w     87.00 178.00   1.00   17.01    --  112.00  33.00 139.00   91
 21  \w     30.00 106.00   1.00   17.01    --  112.00 -95.00 -90.00   76
 22  \w     36.00 109.00   1.00   17.01    --  112.00-111.00 120.00   73
 23  \w     30.00 106.00   1.00   17.01    --  112.00 -95.00  30.00   76
 24  \w     36.00 140.00   1.00   17.01    --  112.00 -30.00  90.00  104
 25  \w     40.00 141.00   1.00   17.01    --  112.00 -61.00-120.00  101
 26  \w    104.00 178.00   1.00   17.01    --  112.00 111.00   0.00   74
 27  \w     61.00 146.00   1.00   17.01    --  112.00 178.00  60.00   85
 28  \w     61.00 146.00   1.00   17.01    --  112.00 178.00  30.00   85
 29  \w     36.00 109.00   1.00   17.01    --  112.00-111.00  90.00   73
 30  \w     36.00 109.00   1.00   17.01    --  112.00-111.00 -30.00   73
 31  \w     40.00 141.00   1.00   17.01    --  112.00 -61.00 120.00  101
 32  \w     40.00 141.00   1.00   17.01    --  112.00 -61.00   0.00  101
 33  \w    103.00 178.00   1.00   17.01    --  112.00  77.00 120.00   75
 34  \w     30.00 165.00   1.00   17.01    --  112.00 -15.00  30.00  135
 35  \w     24.00 178.00   1.00   17.01    --  112.00   0.00-120.00  154
 36  \w    104.00 178.00   1.00   17.01    --  112.00 111.00 -30.00   74
 37  \w     53.00  84.00   1.00   17.01    --  112.00 -95.00 -60.00   31
 38  \w     62.00  88.00   1.00   17.01    --  112.00 -95.00   0.00   26
 39  \w     73.00  99.00   1.00   17.01    --  112.00 -61.00  30.00   26
 40  \w     42.00  68.00   1.00   17.01    --  112.00 -30.00 -30.00   26
 41  \w     76.00 102.00   1.00   17.01    --  112.00 -30.00 -30.00   26
;
_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      0.0467964000
_diffrn_orient_matrix_UB_12      0.1169582000
_diffrn_orient_matrix_UB_13      0.0211342000
_diffrn_orient_matrix_UB_21      0.1578684000
_diffrn_orient_matrix_UB_22      -0.0013944000
_diffrn_orient_matrix_UB_23      0.0373813000
_diffrn_orient_matrix_UB_31      0.0462822000
_diffrn_orient_matrix_UB_32      0.0170113000
_diffrn_orient_matrix_UB_33      -0.0921977000
_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  0.0188
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39179
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.046
_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     666
_refine_ls_number_reflns         7869
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0737P)^2^+0.2209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6376
_reflns_number_total             7869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04614a2.cif
_cod_data_source_block           ka_216_6
_cod_depositor_comments
'Adding full bibliography for 7062847--7062848.cif.'
_cod_database_code               7062848
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H28 Cu F12 N2 O6'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.626
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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. Uiso/Uaniso restraints and constraints
Uanis(F12A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F6)=Sof(F5)=FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(3)
 Sof(F7)=Sof(F9)=Sof(F8)=FVAR(3)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(4)
 Sof(F11)=Sof(F12)=Sof(F10)=FVAR(4)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(5)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(5)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C13(H13), C15(H15), C4(H4), C34(H34), C7(H7), C6(H6),
 C29(H29), C5(H5)
4.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F),
 C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              90067
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.775