Iron(iv) alkyl complexes: electronic structure contributions to Fe-C bond homolysis and migration reactions that form N-C bonds from N<sub>2</sub>.
Bhutto, Samuel M.; Hooper, Reagan X.; McWilliams, Sean F.; Mercado, Brandon Q.; Holland, Patrick L.; Chemical science 15 (2024) 3485–3494; doi:10.1039/d3sc05939a

data_1571368
_publ_section_title
;
 Iron(iv) alkyl complexes: electronic structure contributions to Fe-C bond
 homolysis and migration reactions that form N-C bonds from N<sub>2</sub>.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3485
_journal_page_last               3494
_journal_paper_doi               10.1039/d3sc05939a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '	C36 H48 Fe N2, C20 H40 K O8'
_chemical_formula_sum            'C56 H88 Fe K N2 O8'
_chemical_formula_weight         1012.23
_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
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-13 deposited with the CCDC.	2024-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                83.732(3)
_cell_angle_beta                 71.934(4)
_cell_angle_gamma                66.707(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0503(6)
_cell_length_b                   13.4395(6)
_cell_length_c                   20.4096(7)
_cell_measurement_reflns_used    34589
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.6690
_cell_measurement_theta_min      2.1600
_cell_volume                     3125.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112250
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.559
_diffrn_reflns_theta_max         66.559
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    2.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.585
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1219P)^2^+3.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8540
_reflns_number_total             10888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05939a2.cif
_cod_data_source_block           007a-21112
_cod_database_code               1571368
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.595
_shelx_estimated_absorpt_t_max   0.760
_shelx_res_checksum              40025
_shelx_fab_checksum              21143