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_7246149
_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         'C20 H30 Co, C36 H27 N3 O6'
_chemical_formula_sum            'C56 H57 Co N3 O6'
_chemical_formula_weight         926.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.711(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8607(12)
_cell_length_b                   18.4970(7)
_cell_length_c                   12.9906(6)
_cell_measurement_reflns_used    8924
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.2040
_cell_measurement_theta_min      3.4780
_cell_volume                     4655.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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 0.992
_diffrn_measured_fraction_theta_max 0.862
_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    -10.00  16.00   0.50   82.85    --   -0.90  45.00 150.00   52
  2  \w    -48.00 -15.00   0.50   82.85    --   -0.90  45.00  30.00   66
  3  \w    -86.00  88.00   0.50   82.85    --   -0.90  45.00  60.00  348
  4  \w      7.00  19.50   0.50   82.85    --   -0.90  45.00   0.00   25
;
_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      -0.0103322000
_diffrn_orient_matrix_UB_12      -0.0229668000
_diffrn_orient_matrix_UB_13      -0.0443803000
_diffrn_orient_matrix_UB_21      -0.0142794000
_diffrn_orient_matrix_UB_22      0.0301026000
_diffrn_orient_matrix_UB_23      -0.0310282000
_diffrn_orient_matrix_UB_31      0.0320809000
_diffrn_orient_matrix_UB_32      0.0062528000
_diffrn_orient_matrix_UB_33      -0.0140495000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27034
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.860
_diffrn_reflns_theta_min         2.727
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+6.6498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4835
_reflns_number_total             6898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp06026d2.cif
_cod_data_source_block           220630codmcp2bti-xy
_cod_depositor_comments
'Adding full bibliography for 7246148--7246150.cif.'
_cod_database_code               7246149
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCo
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.848
_diffrn_oxdiff_digest_frames
;
01f62ce7f4df29321e342bc565ccb2a64f000251e1f
;
_diffrn_oxdiff_digest_hkl
;
01c58cb6abc69875f1395fb79635017810b284
;
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00R(H00R), C00T(H00T), C00X(H00X)
2.b Idealised Me refined as rotating group:
 C00H(H00A,H00B,H00C), C00I(H00J,H00K,H00M), C00Q(H00D,H00E,H00F), C00U(H00G,
 H00H,H00I), C00V(H00O,H00P,H00Q), C00W(H00S,H00U,H00V), C00Y(H00W,H00Y,H),
 C00Z(H00Z,HA,HB)
;
_shelx_res_checksum              84420
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.775