Stabilization of a high-spin three-coordinate Fe(iii) imidyl complex by radical delocalization
Yang, Po-Chun; Yu, Kuan-Po; Hsieh, Chi-Tien; Zou, Junjie; Fang, Chia-Te; Liu, Hsin-Kuan; Pao, Chih-Wen; Deng, Liang; Cheng, Mu-Jeng; Lin, Chun-Yi; Chemical Science 13 (2022) 9637–9643; doi:10.1039/D2SC02699F

data_1567442
_publ_section_title
;
 Stabilization of a high-spin three-coordinate Fe(iii) imidyl complex by
 radical delocalization
;
_journal_issue                   33
_journal_name_full               'Chemical Science'
_journal_page_first              9637
_journal_page_last               9643
_journal_paper_doi               10.1039/D2SC02699F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_sum            'C41 H63 Fe N3'
_chemical_formula_weight         653.79
_chemical_properties_physical
'Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Metastable as a solid and in solution'
_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_method           SHELXL-2018/3
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                104.6620(10)
_cell_angle_beta                 92.2470(10)
_cell_angle_gamma                90.1830(10)
_cell_formula_units_Z            4
_cell_length_a                   9.6054(3)
_cell_length_b                   19.7203(6)
_cell_length_c                   20.7848(6)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.31
_cell_volume                     3805.6(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            103949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.172
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         18940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+2.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16307
_reflns_number_total             18940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02699f2.cif
_cod_data_source_block           21JUN11_1_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567442--1567445.cif.'
_cod_database_code               1567442
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              39549