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_1567091
_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, C18 H36 K N2 O6'
_chemical_formula_sum            'C57 H99 Fe K N5 O6 Si2'
_chemical_formula_weight         1101.54
_chemical_name_systematic        K{crypt}[Fe(NMes)(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                 95.9740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9424(4)
_cell_length_b                   24.7899(9)
_cell_length_c                   22.9964(9)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.37
_cell_volume                     6771.1(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85806
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.961
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   none
_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            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             2388
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         16789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0402P)^2^+5.3159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13838
_reflns_number_total             16789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01088g2.cif
_cod_data_source_block           k_crypt_1
_cod_depositor_comments
'Adding full bibliography for 1567091--1567094.cif.'
_cod_database_code               1567091
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.927
_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:
 C00M(H00M), C00S(H00S), C00Z(H00Z), C013(H013)
2.b Secondary CH2 refined with riding coordinates:
 C010(H6,H), C011(H7,HA), C014(H8,HB), C016(H9,HC), C017(H10,HD), C018(H11,HE),
  C019(H12,HF), C01B(H13,HG), C01C(H14,HH), C01D(H15,HI), C01E(H16,HJ),
 C01F(H17,HK), C01G(H18,HL), C01I(H19,HM), C01L(H20,HN), C01M(H21,HO), C01T(H22,
 HV), C01W(H23,H24)
2.c Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00Q(H00Q), C00R(H00R), C00T(H00T), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C012(H012)
2.d Idealised Me refined as rotating group:
 C015(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01H(H01G,H01H,H01I), C01J(H01J,
 H01K,H01L), C01K(H01M,H01N,H01O), C01N(H01P,H01Q,H01R), C01O(H01S,H01T,H01U),
 C01P(H01V,H01W,H01X), C01Q(H01Y,HP,HQ), C01R(H01Z,HR,HS), C01S(H01,HT,HU),
 C01U(H1,HW,HX), C01V(H2,HY,HZ), C01X(H3,H25,H26), C01Y(H4,H27,H28), C01Z(H5,
 H29,H30), C020(H02A,H02B,H02C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7640
_shelx_hkl_checksum              19747
_shelx_fab_checksum              21075
_olex2_submission_special_instructions 'No special instructions were received'