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_1567094
_publ_section_title
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 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         'C40 H63 Fe N3 S2 Si2, C18 H36 K N2 O6'
_chemical_formula_sum            'C58 H99 Fe K N5 O6 S2 Si2'
_chemical_formula_weight         1177.67
_chemical_name_systematic        K{crypt}[Fe(S2CNMes)(N{Dipp}TMS)2]
_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
_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                 90.755(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8538(8)
_cell_length_b                   24.6616(14)
_cell_length_c                   23.5229(13)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.21
_cell_volume                     8036.1(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_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  0.1409
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            237874
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.904
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1637 before and 0.0874 after correction. The Ratio of minimum to maximum transmission is 0.7917. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         14145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+6.3339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10618
_reflns_number_total             14145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01088g2.cif
_cod_data_source_block           k_crypt_2
_cod_depositor_comments
'Adding full bibliography for 1567091--1567094.cif.'
_cod_database_code               1567094
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C26(H26), C36(H36), C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C52(H52A,H52B), C15(H15A,H15B), C33(H33A,H33B), C17(H17A,
 H17B), C9(H9A,H9B), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B), C3(H3A,
 H3B), C49(H49A,H49B), C25(H25A,H25B), C51(H51A,H51B), C13(H13A,H13B), C53(H53A,
 H53B), C27(H27A,H27B), C55(H55A,H55B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C30(H30), C32(H32), C34(H34), C38(H38), C44(H44), C58(H58), C35(H35)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C56(H56A,H56B,H56C), C31(H31A,
 H31B,H31C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C),
 C5(H5A,H5B,H5C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C),
  C23(H23A,H23B,H23C), C57(H57A,H57B,H57C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87188
_shelx_hkl_checksum              70666
_shelx_fab_checksum              17989
_olex2_submission_special_instructions 'No special instructions were received'