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_7246148
_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         'C36 H27 N3 O6, C7'
_chemical_formula_sum            'C43 H27 N3 O6'
_chemical_formula_weight         681.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-12
_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                 105.010(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8004(4)
_cell_length_b                   18.9270(6)
_cell_length_c                   11.5824(4)
_cell_measurement_reflns_used    10138
_cell_measurement_temperature    300
_cell_measurement_theta_max      31.8770
_cell_measurement_theta_min      3.5650
_cell_volume                     1863.40(13)
_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      300
_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 0.997
_diffrn_measured_fraction_theta_max 0.889
_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    -68.00 -42.00   0.50   18.00    --    0.00  45.00   0.00   52
  2  \w    -31.00  -5.00   0.50   18.00    --    0.00  45.00   0.00   52
  3  \w     27.00  89.00   0.50   18.00    --    0.00  45.00   0.00  124
  4  \w    -36.00 -10.00   0.50   18.00    --    0.00  45.00  60.00   52
  5  \w    -89.00  68.00   0.50   18.00    --    0.00  45.00  90.00  314
;
_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      0.0208877000
_diffrn_orient_matrix_UB_12      -0.0023343000
_diffrn_orient_matrix_UB_13      -0.0550707000
_diffrn_orient_matrix_UB_21      0.0802305000
_diffrn_orient_matrix_UB_22      -0.0039471000
_diffrn_orient_matrix_UB_23      0.0314503000
_diffrn_orient_matrix_UB_31      -0.0098766000
_diffrn_orient_matrix_UB_32      -0.0371699000
_diffrn_orient_matrix_UB_33      -0.0001186000
_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  0.0195
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26955
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.797
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66298
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       needle
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0942P)^2^+0.2616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4537
_reflns_number_total             5799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp06026d2.cif
_cod_data_source_block           211111bti-xy
_cod_depositor_comments
'Adding full bibliography for 7246148--7246150.cif.'
_cod_database_code               7246148
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.984
_diffrn_oxdiff_digest_frames
;
0170a54f1e6e7bfd61e1205c6268deb7a400025ea60
;
_diffrn_oxdiff_digest_hkl
;
01fb13bac67c8f64bed41379bcf9e6113ac16d
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C23(0.5) C22(0.5) C26(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,
 H1BC)
;
_shelx_res_checksum              51
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.663