Slow magnetic relaxation and spin crossover behavior in two mixed-valence Co(ii)/Co(iii) complexes
Huang, You-Lin; Zhong, Yun-Jing; Ye, Hua-Jian; Li, You-Hong; Kuang, Xiao-Man; Ouyang, Zhi-Jian; Chen, Wen-Bin; Yang, Meng; Dong, Wen; New Journal of Chemistry 46 (2022) 17720–17725; doi:10.1039/D2NJ03051A

data_7061756
_publ_section_title
;
 Slow magnetic relaxation and spin crossover behavior in two mixed-valence
 Co(ii)/Co(iii) complexes
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17720
_journal_page_last               17725
_journal_paper_doi               10.1039/D2NJ03051A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C30 H22 Co N6, 2(C22 H12 Co N12 O4)'
_chemical_formula_sum            'C90 H84 Co3 N34 O13'
_chemical_formula_weight         2026.70
_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
_audit_creation_date             2022-08-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-19 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                77.152(3)
_cell_angle_beta                 80.333(3)
_cell_angle_gamma                73.050(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5085(4)
_cell_length_b                   15.2210(9)
_cell_length_c                   28.5790(6)
_cell_measurement_reflns_used    31461
_cell_measurement_temperature    297.99(18)
_cell_measurement_theta_max      76.2840
_cell_measurement_theta_min      3.1090
_cell_volume                     4640.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_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    -17.00  30.00   0.50    0.40    --  -45.87  22.00  97.00   94
  2  \w    -38.00  22.00   0.50    0.40    --  -45.87  37.00 -30.00  120
  3  \w    -25.00  25.00   0.50    0.40    --  -45.87  19.00-120.00  100
  4  \w    -25.00  30.00   0.50    0.40    --  -45.87  19.00-180.00  110
  5  \w     -5.00  25.00   0.50    0.40    --   45.87 -22.00 -68.00   60
  6  \w     38.00  67.00   0.50    1.59    --  106.06 -61.00-120.00   58
  7  \w     37.00  66.00   0.50    1.59    --  106.06 -61.00-180.00   58
  8  \w     70.00  96.00   0.50    1.59    --  106.06 -94.00-180.00   52
  9  \w     44.00 106.00   0.50    1.59    --  106.06 -94.00 -90.00  124
 10  \w     86.00 111.00   0.50    1.59    --  106.06-125.00 -30.00   50
 11  \w     73.00 112.00   0.50    1.59    --  106.06-125.00 -60.00   78
 12  \w     68.00 105.00   0.50    1.59    --  106.06 -94.00  30.00   74
 13  \w     69.00 112.00   0.50    1.59    --  106.06-125.00  60.00   86
 14  \w     79.00 105.00   0.50    1.59    --  106.06 -94.00 120.00   52
 15  \w     35.00  72.00   0.50    1.59    --  106.06-125.00  30.00   74
 16  \w     43.00  75.00   0.50    1.59    --  106.06-125.00 -30.00   64
 17  \w     47.00  94.00   0.50    1.59    --  106.06 -94.00 -30.00   94
 18  \w     36.00  96.00   0.50    1.59    --  106.06 -94.00  60.00  120
 19  \w     33.00  58.00   0.50    1.59    --  106.06-125.00 -60.00   50
 20  \w     68.00  93.00   0.50    0.40    --   45.87-125.00-180.00   50
 21  \w     34.00  66.00   0.50    1.59    --  106.06 -94.00-180.00   64
 22  \w     91.00 178.00   0.50    1.59    --  106.06  30.00-180.00  174
 23  \w    143.00 176.00   0.50    1.59    --  106.06 125.00 -30.00   66
 24  \w     83.00 109.00   0.50    0.40    --   45.87  22.00  97.00   52
 25  \w     92.00 147.00   0.50    1.59    --  106.06  22.00  97.00  110
 26  \w    126.00 175.00   0.50    1.59    --  106.06  30.00 150.00   98
 27  \w     91.00 165.00   0.50    1.59    --  106.06  61.00  90.00  148
 28  \w     90.00 122.00   0.50    1.59    --  106.06 125.00 -30.00   64
 29  \w     91.00 163.00   0.50    1.59    --  106.06  77.00-150.00  144
 30  \w     34.00  80.00   0.50    0.40    --   45.87  22.00  97.00   92
 31  \w     35.00  72.00   0.50    1.59    --  106.06 -61.00 150.00   74
 32  \w     36.00  61.00   0.50    1.59    --  106.06-125.00  60.00   50
 33  \w    -93.00 -31.00   0.50    0.40    --  -45.87 -22.00 -68.00  124
 34  \w   -118.00 -92.00   0.50    0.40    --  -45.87-125.00 120.00   52
 35  \w   -132.00 -74.00   0.50    1.59    -- -102.00-125.00  30.00  116
 36  \w   -155.00 -87.00   0.50    1.59    -- -102.00 -45.00  60.00  136
 37  \w   -170.00 -87.00   0.50    1.59    -- -102.00 -22.00 -68.00  166
 38  \w   -171.00-142.00   0.50    1.59    -- -102.00-125.00  30.00   58
 39  \w    -65.00 -35.00   0.50    1.59    -- -102.00 107.00-160.24   60
 40  \w    -65.00 -30.00   0.50    1.59    -- -102.00 110.00 -74.34   70
 41  \w    -71.00 -22.00   0.50    0.40    --  -45.87 125.00 -90.00   98
 42  \w    -76.00 -31.00   0.50    1.59    -- -102.00 125.00  30.00   90
 43  \w    -91.00 -51.00   0.50    0.40    --  -45.87 125.00 150.00   80
 44  \w   -110.00 -31.00   0.50    1.59    -- -102.00 125.00  90.00  158
 45  \w   -108.00 -82.00   0.50    1.59    -- -102.00 110.00 -74.34   52
 46  \w   -107.00 -81.00   0.50    1.59    -- -102.00 107.00-160.24   52
 47  \w   -108.00 -35.00   0.50    1.59    -- -102.00 109.00  -7.31  146
 48  \w   -128.00 -68.00   0.50    1.59    -- -102.00 148.00  50.80  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63067
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.349
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    4.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             2094
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00030(6)
_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   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         18771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0534
_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^)+(0.1099P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15182
_reflns_number_total             18771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03051a2.cif
_cod_data_source_block           co-298k
_cod_depositor_comments
'Adding full bibliography for 7061754--7061757.cif.'
_cod_database_code               7061756
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.445
_shelx_estimated_absorpt_t_min   0.325
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
 C37(H37), C38(H38), C40(H40), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51),
  C56(H56), C57(H57), C59(H59), C60(H60), C62(H62), C67(H67), C68(H68),
 C70(H70), C71(H71), C73(H73)
2.b Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O4(H4A), O6(H6), O8(H8A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95717
_shelx_fab_checksum              46285
_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
;