Observation of slow magnetic relaxation phenomena in spatially isolated π-radical ions.
Koyama, Shohei; Sato, Kazunobu; Yamashita, Masahiro; Sakamoto, Ryota; Iguchi, Hiroaki; Physical chemistry chemical physics : PCCP 25 (2023) 5459–5467; doi:10.1039/d2cp06026d

data_7246150
_publ_section_title
;
 Observation of slow magnetic relaxation phenomena in spatially isolated
 &#x3c0;-radical ions.
;
_journal_issue                   7
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              5459
_journal_page_last               5467
_journal_paper_doi               10.1039/d2cp06026d
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C10 Co1, C36 H27 N3 O6'
_chemical_formula_sum            'C46 H27 Co N3 O6'
_chemical_formula_weight         776.63
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.8716(2)
_cell_length_b                   13.8716(2)
_cell_length_c                   33.7979(8)
_cell_measurement_reflns_used    23278
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.9240
_cell_measurement_theta_min      3.5730
_cell_volume                     5632.14(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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      120
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_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     53.00  79.00   0.50    7.50    --   -0.30  45.00 179.42   52
  2  \w    -45.00  -4.00   0.50    7.50    --   -0.30  45.00  60.00   82
  3  \w     64.00  89.00   0.50    7.50    --   -0.30  45.00  60.00   50
  4  \w    -73.00 -47.00   0.50    7.50    --   -0.30  45.00 120.00   52
  5  \w     -5.00  29.00   0.50    7.50    --   -0.30  45.00 120.00   68
  6  \w    -89.00  75.00   0.50    7.50    --   -0.30  45.00   0.00  328
  7  \w    -71.00  89.00   0.50    7.50    --   -0.30  45.00  90.00  320
  8  \w    -21.00   4.00   0.50    7.50    --   -0.30  45.00  30.00   50
  9  \w      4.00  29.00   0.50    7.50    --   -0.30  45.00 150.00   50
 10  \w    -32.00   2.00   0.50    7.50    --   -0.30  45.00 179.42   68
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0183551333
_diffrn_orient_matrix_UB_12      0.0389539333
_diffrn_orient_matrix_UB_13      0.0028363333
_diffrn_orient_matrix_UB_21      -0.0551218667
_diffrn_orient_matrix_UB_22      -0.0443753333
_diffrn_orient_matrix_UB_23      0.0030315667
_diffrn_orient_matrix_UB_31      0.0106140667
_diffrn_orient_matrix_UB_32      0.0012811333
_diffrn_orient_matrix_UB_33      0.0205632333
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0089
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            48222
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.804
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             2394
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+9.0551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1848
_reflns_number_total             2079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp06026d2.cif
_cod_data_source_block           210915cocp2_bti-xy
_cod_depositor_comments
'Adding full bibliography for 7246148--7246150.cif.'
_cod_original_cell_volume        5632.1(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7246150
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCo
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.821
_diffrn_oxdiff_digest_frames
;
01b112c73ed7f5b689c45cced229d91699011203063
;
_diffrn_oxdiff_digest_hkl
;
0199c0c7e53fbb23035da026c5f026df71a458
;
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H3 of C3, H14 of C14
 At 1.2 times of:
  H13 of C13
2. Others
 Fixed Sof: C12(0.5) C2(0.83333) C14(0.5) H14(0.5) C13(0.5) H13(0.5) C4(0.5)
 C3(0.5) H3(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) C6(0.41667) C8(0.41667)
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              89203
_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 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.689