Field supported slow magnetic relaxation in a quasi-one-dimensional copper(ii) complex with a pentaheterocyclic triphenodioxazine
Korchagin, D. V.; Ivakhnenko, E. P.; Demidov, O. P.; Akimov, A. V.; Morgunov, R. B.; Starikov, A. G.; Palii, A. V.; Minkin, V. I.; Aldoshin, S. M.; New Journal of Chemistry 45 (2021) 21912–21918; doi:10.1039/D1NJ03217H

data_7061030
_publ_section_title
;
 Field supported slow magnetic relaxation in a quasi-one-dimensional
 copper(ii) complex with a pentaheterocyclic triphenodioxazine
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21912
_journal_page_last               21918
_journal_paper_doi               10.1039/D1NJ03217H
_journal_volume                  45
_journal_year                    2021
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_moiety         '2(C5 H Cu0.5 F6 O2), C26 H25 Cl N2 O2'
_chemical_formula_sum            'C36 H27 Cl Cu F12 N2 O6'
_chemical_formula_weight         910.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-30 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.745(2)
_cell_angle_beta                 97.906(2)
_cell_angle_gamma                105.700(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4631(2)
_cell_length_b                   13.7164(3)
_cell_length_c                   15.5325(3)
_cell_measurement_reflns_used    11750
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8930
_cell_measurement_theta_min      4.2330
_cell_volume                     1917.60(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.994
_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    4.00    --  -41.72 -57.00-120.00  100
  2  \w   -116.00 -17.00   1.00    4.00    --  -41.72 -38.00 120.00   99
  3  \w    -70.00  31.00   1.00    4.00    --  -41.72  57.00  30.00  101
  4  \w      7.00  34.00   1.00    4.00    --   41.72  83.00  60.20   27
  5  \w      8.00  42.00   1.00    4.00    --   41.72  81.00-130.07   34
  6  \w    -21.00  74.00   1.00    4.00    --   41.72 -77.00  90.00   95
  7  \w     36.00 109.00   1.00   16.00    --  112.00-111.00 120.00   73
  8  \w     36.00 145.00   1.00   16.00    --  112.00 -77.00  30.00  109
  9  \w     28.00 178.00   1.00   16.00    --  112.00  -9.00 -18.39  150
 10  \w     36.00 109.00   1.00   16.00    --  112.00-111.00  90.00   73
 11  \w     36.00 140.00   1.00   16.00    --  112.00 -30.00  60.00  104
 12  \w     30.00 106.00   1.00   16.00    --  112.00 -95.00 -30.00   76
 13  \w     30.00 106.00   1.00   16.00    --  112.00 -95.00  30.00   76
 14  \w     40.00 141.00   1.00   16.00    --  112.00 -61.00  30.00  101
 15  \w     39.00 138.00   1.00   16.00    --  112.00 -45.00 150.00   99
 16  \w     36.00 109.00   1.00   16.00    --  112.00-111.00-120.00   73
 17  \w     36.00 109.00   1.00   16.00    --  112.00-111.00 -60.00   73
 18  \w     36.00 109.00   1.00   16.00    --  112.00-111.00   0.00   73
 19  \w     36.00 140.00   1.00   16.00    --  112.00 -30.00-120.00  104
 20  \w     36.00 109.00   1.00   16.00    --  112.00-111.00-150.00   73
 21  \w     36.00 109.00   1.00   16.00    --  112.00-111.00  30.00   73
 22  \w     86.00 178.00   1.00   16.00    --  112.00  45.00 -90.00   92
 23  \w     30.00 106.00   1.00   16.00    --  112.00 -95.00 120.00   76
 24  \w    104.00 178.00   1.00   16.00    --  112.00 111.00   0.00   74
 25  \w     36.00 140.00   1.00   16.00    --  112.00 -30.00-180.00  104
 26  \w     86.00 178.00   1.00   16.00    --  112.00  45.00 -30.00   92
 27  \w     61.00 146.00   1.00   16.00    --  112.00 178.00 -60.00   85
 28  \w     36.00 109.00   1.00   16.00    --  112.00-111.00 -30.00   73
 29  \w     40.00 141.00   1.00   16.00    --  112.00 -61.00  90.00  101
 30  \w     36.00 145.00   1.00   16.00    --  112.00 -77.00 -90.00  109
 31  \w     36.00 109.00   1.00   16.00    --  112.00-111.00-180.00   73
 32  \w    104.00 178.00   1.00   16.00    --  112.00 111.00 -60.00   74
 33  \w     30.00 106.00   1.00   16.00    --  112.00 -95.00 150.00   76
 34  \w     83.00 178.00   1.00   16.00    --  112.00  61.00-180.00   95
 35  \w     40.00 141.00   1.00   16.00    --  112.00 -61.00 -30.00  101
 36  \w     40.00 141.00   1.00   16.00    --  112.00 -61.00 150.00  101
 37  \w     36.00 145.00   1.00   16.00    --  112.00 -77.00-150.00  109
 38  \w     84.00 137.00   1.00   16.00    --  112.00 -34.00 -67.69   53
 39  \w     73.00  98.00   1.00    4.00    --   41.60-125.00-120.00   25
 40  \w     63.00  89.00   1.00   16.00    --  112.00 -36.00 161.35   26
 41  \w    142.00 167.00   1.00   16.00    --  112.00   6.00  59.62   25
 42  \w    107.00 133.00   1.00   16.00    --  112.00 111.00-150.00   26
 43  \w    149.00 175.00   1.00   16.00    --  112.00 111.00-150.00   26
 44  \w     30.00  76.00   1.00   16.00    --  112.00   6.00  59.62   46
 45  \w    129.00 154.00   1.00   16.00    --  112.00  77.00 -60.00   25
 46  \w     79.00 105.00   1.00   16.00    --  112.00 178.00   0.00   26
 47  \w    121.00 146.00   1.00   16.00    --  112.00 178.00   0.00   25
 48  \w    104.00 146.00   1.00   16.00    --  112.00  45.00-150.00   42
 49  \w     67.00  92.00   1.00   16.00    --  112.00 -61.00 -60.00   25
 50  \w     97.00 123.00   1.00   16.00    --  112.00  45.00  90.00   26
 51  \w    120.00 146.00   1.00   16.00    --  112.00  45.00 120.00   26
 52  \w     79.00 105.00   1.00   16.00    --  112.00 -79.00  12.18   26
 53  \w    123.00 149.00   1.00   16.00    --  112.00  77.00  30.00   26
 54  \w     53.00  79.00   1.00   16.00    --  112.00 -95.00   0.00   26
 55  \w     99.00 146.00   1.00   16.00    --  112.00  45.00   0.00   47
 56  \w     89.00 115.00   1.00   16.00    --  112.00  61.00  90.00   26
 57  \w     47.00  73.00   1.00   16.00    --  112.00 -61.00 120.00   26
 58  \w     74.00 100.00   1.00   16.00    --  112.00 -66.00 -94.04   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400800000
_diffrn_orient_matrix_UB_12      0.0881911000
_diffrn_orient_matrix_UB_13      -0.0473287000
_diffrn_orient_matrix_UB_21      0.0972188000
_diffrn_orient_matrix_UB_22      0.0757600000
_diffrn_orient_matrix_UB_23      0.0742282000
_diffrn_orient_matrix_UB_31      0.1349472000
_diffrn_orient_matrix_UB_32      0.0127714000
_diffrn_orient_matrix_UB_33      -0.0482494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.524
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         8016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0693P)^2^+0.4813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5990
_reflns_number_total             8016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03217h2.cif
_cod_data_source_block           ka_185_2
_cod_depositor_comments          'Adding full bibliography for 7061030.cif.'
_cod_database_code               7061030
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H27 Cl Cu F12 N2 O6'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.564
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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(F22) = Uanis(F24) = Uanis(F23)
Uanis(F5) = Uanis(F6) = Uanis(F2)
3. Others
 Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F2)=1-FVAR(2)
 Sof(F1)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(F9)=Sof(F12)=1-FVAR(3)
 Sof(F8)=Sof(F11)=FVAR(3)
 Sof(F10)=1-FVAR(4)
 Sof(F7)=FVAR(4)
 Sof(F24)=Sof(F22)=Sof(F23)=1-FVAR(5)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(5)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(6)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(6)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C16(H16), C13(H13), C4(H4), C2(H2), C10(H10), C30(H30), C11(H11),
 C35(H35)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C28(H28A,H28B,
 H28C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              91103
_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 1.596
_oxdiff_exptl_absorpt_empirical_full_min 0.769