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_1567443
_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            'C32 H52 Li2 N2'
_chemical_formula_weight         478.63
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
;
2021-11-15 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                74.635(3)
_cell_angle_beta                 87.557(3)
_cell_angle_gamma                62.337(2)
_cell_formula_units_Z            1
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_cell_length_b                   9.3153(5)
_cell_length_c                   10.4649(6)
_cell_measurement_reflns_used    4759
_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      2.57
_cell_volume                     745.10(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6982
_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            green
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       bulk
_exptl_crystal_F_000             264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.296
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_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0636P)^2^+0.4272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2878
_reflns_number_total             3697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02699f2.cif
_cod_data_source_block           20DEC20
_cod_depositor_comments
'Adding full bibliography for 1567442--1567445.cif.'
_cod_database_code               1567443
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              67559