Between imide, imidyl and nitrene - an imido iron complex in two oxidation states.
Reith, Sascha; Demeshko, Serhiy; Battistella, Beatrice; Reckziegel, Alexander; Schneider, Christian; Stoy, Andreas; Lichtenberg, Crispin; Meyer, Franc; Munz, Dominik; Werncke, C. Gunnar; Chemical science 13 (2022) 7907–7913; doi:10.1039/d2sc01088g

data_1567092
_publ_section_title
;
 Between imide, imidyl and nitrene - an imido iron complex in two
 oxidation states.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7907
_journal_page_last               7913
_journal_paper_doi               10.1039/d2sc01088g
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C39 H63 Fe N3 Si2'
_chemical_formula_sum            'C39 H63 Fe N3 Si2'
_chemical_formula_weight         685.95
_chemical_name_systematic        '[Fe(NMes)(N{Dipp}TMS)2]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6372)
;
_audit_update_record
;
2021-12-22 deposited with the CCDC.	2022-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2646(7)
_cell_length_b                   16.7587(7)
_cell_length_c                   24.9520(11)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.29
_cell_volume                     8055.7(6)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            76439
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.945
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0260P)^2^+8.7490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             7090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01088g2.cif
_cod_data_source_block           fenmes_1
_cod_depositor_comments
'Adding full bibliography for 1567091--1567094.cif.'
_cod_database_code               1567092
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.904
_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.a Ternary CH refined with riding coordinates:
 C32(H32), C34(H34), C5(H5), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C20(H20), C26(H26), C28(H28), C36(H36), C39(H39), C13(H13), C27(H27)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C21(H21A,H21B,H21C), C11(H11A,H11B,
 H11C), C3(H3A,H3B,H3C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C29(H29A,H29B,
 H29C), C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C33(H33A,
 H33B,H33C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C), C9(H9A,H9B,H9C),
 C37(H37A,H37B,H37C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              21976
_shelx_hkl_checksum              51378
_olex2_submission_special_instructions 'No special instructions were received'