Spectroscopic and thermodynamic characterization of a cobalt-verdazyl valence tautomeric system. influence of crystal structure, solvent and counterion.
Brook, David J. R.; DaRos, Jeffrey; Ponnekanti, Aamani; Agrestini, Stefano; Pellegrin, Eric; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7536–7545; doi:10.1039/d4dt00465e

data_7715613
_publ_section_title
;
 Spectroscopic and thermodynamic characterization of a cobalt-verdazyl
 valence tautomeric system. influence of crystal structure, solvent and
 counterion.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7536
_journal_page_last               7545
_journal_paper_doi               10.1039/d4dt00465e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H30 Co N12 O2, 2(B F4)'
_chemical_formula_sum            'C30 H30 B2 Co F8 N12 O2'
_chemical_formula_weight         823.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-14 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0663(16)
_cell_length_b                   17.1914(18)
_cell_length_c                   29.810(7)
_cell_measurement_reflns_used    2125
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.7060
_cell_measurement_theta_min      2.6270
_cell_volume                     6696.2(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      0.00  98.00   1.00   60.00    --   25.41  37.00-180.00   98
  2  \w    -20.00  67.00   1.00   60.00    --   25.41 -99.00 -60.00   87
  3  \w    -96.00  -6.00   1.00   60.00    --  -27.28 -57.00 -60.00   90
  4  \w    -49.00  42.00   1.00   60.00    --  -27.28  57.00   0.00   91
  5  \w    -96.00 -60.00   1.00   60.00    --  -27.28 -57.00-150.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11728
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.073
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.92869
_exptl_absorpt_correction_T_min  0.92869
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
;
_exptl_crystal_colour            'lustrous black'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.089
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0844
_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^)+(0.0474P)^2^+98.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1250
_reflns_number_total             1726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00465e2.cif
_cod_data_source_block           db30b_3
_cod_depositor_comments
'Adding full bibliography for 7715611--7715614.cif.'
_cod_original_cell_volume        6696.2(18)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7715613
_shelx_shelxl_version_number     2018/3
_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(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O1(0.5) N1(0.5) N2(0.5) N3(0.5) N4(0.5) C1(0.5) C2(0.5) C3(0.5)
 H3(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              7465
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;