A homoleptic Fe(iv) ketimide complex with a low-lying excited state.
Hertler, Phoebe R.; Sauza-de la Vega, Arturo; Darù, Andrea; Sarkar, Arup; Lewis, Richard A.; Wu, Guang; Gagliardi, Laura; Hayton, Trevor W.; Chemical science 15 (2024) 16559–16566; doi:10.1039/d4sc04880f

data_1572554
_publ_section_title
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 A homoleptic Fe(iv) ketimide complex with a low-lying excited state.
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_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16559
_journal_page_last               16566
_journal_paper_doi               10.1039/d4sc04880f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C52 H76 Fe Li2 N4 O2'
_chemical_formula_weight         858.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-04-07 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.142(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.334(5)
_cell_length_b                   13.388(4)
_cell_length_c                   23.028(9)
_cell_measurement_reflns_used    8616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.31
_cell_volume                     5521(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39849
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.137
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0066(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+7.6576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             9402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04880f2.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 1572554--1572556.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1572554
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              19770
_shelx_hkl_checksum              64681