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_1567093
_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         'C30 H52 Fe N2 Si2, C18 H36 K N2 O6'
_chemical_formula_sum            'C48 H88 Fe K N4 O6 Si2'
_chemical_formula_weight         968.35
_chemical_name_systematic        K{crypt}[Fe(N{Dipp}TMS)2]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 106.2980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2810(8)
_cell_length_b                   14.0555(6)
_cell_length_c                   22.1239(9)
_cell_measurement_reflns_used    9738
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.40
_cell_volume                     5456.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  "'Bruker D8 Quest"
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            114411
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.795
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1478 before and 0.0527 after correction. The Ratio of minimum to maximum transmission is 0.9254. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       plate
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.411
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11654
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0396P)^2^+6.2187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9733
_reflns_number_total             11654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01088g2.cif
_cod_data_source_block           k_crypt_fendipptms
_cod_depositor_comments
'Adding full bibliography for 1567091--1567094.cif.'
_cod_database_code               1567093
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.809
_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. Restrained distances
 K1-O009 \\sim K1-O0
 with sigma of 0.02
 K1-O00M \\sim K1-O00N
 with sigma of 0.02
 O009-C00Q \\sim O0-C0AA
 with sigma of 0.02
 O009-C01I \\sim O0-C1AA
 with sigma of 0.02
 N3-C015 \\sim N3-C0
 with sigma of 0.02
 N4-C01D \\sim N4-C3AA
 with sigma of 0.02
 O00M-C01C \\sim O00N-C2AA
 with sigma of 0.02
 O00M-C01R \\sim O00N-C01S
 with sigma of 0.02
 C00Q-C015 \\sim C0AA-C0
 with sigma of 0.02
 C01C-C01D \\sim C2AA-C3AA
 with sigma of 0.02
 C01I-C01R \\sim C1AA-C01S
 with sigma of 0.02
 K1-C00Q \\sim K1-C0AA
 with sigma of 0.04
 K1-C01C \\sim K1-C2AA
 with sigma of 0.04
 K1-C01I \\sim K1-C1AA
 with sigma of 0.04
 K1-C01R \\sim K1-C01S
 with sigma of 0.04
 O009-C015 \\sim O0-C0
 with sigma of 0.04
 O009-C01R \\sim O0-C01S
 with sigma of 0.04
 N3-C00Q \\sim N3-C0AA
 with sigma of 0.04
 N4-C01C \\sim N4-C2AA
 with sigma of 0.04
 O00M-C01D \\sim O00N-C3AA
 with sigma of 0.04
 O00M-C01I \\sim O00N-C1AA
 with sigma of 0.04
 C00Q-C01I \\sim C0AA-C1AA
 with sigma of 0.04
 C01C-C01R \\sim C2AA-C01S
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C015) = Uanis(C00Q) = Uanis(C01I) = Uanis(C01R) = Uanis(C01C) =
Uanis(C01D) = Uanis(C01F) = Uanis(C00W) = Uanis(C00P) = Uanis(C00V) =
Uanis(C00S) = Uanis(C01A) = Uanis(C011) = Uanis(C014) = Uanis(C013) =
Uanis(C00Y) = Uanis(C012) = Uanis(C01H)
Uanis(O009) = Uanis(O00M) = Uanis(O007) = Uanis(C00P) = Uanis(O005) =
Uanis(O008) = Uanis(O006)
4. Others
 Fixed Sof: O009(0.5) O00M(0.5) C00Q(0.5) H00F(0.5) H00I(0.5) C015(0.5)
 H7(0.5) HD(0.5) C01C(0.5) H9(0.5) HF(0.5) C01D(0.5) H10(0.5) HG(0.5) C01I(0.5)
 H13(0.5) HJ(0.5) C01R(0.5) H14(0.5) HU(0.5) C0(0.5) H0A(0.5) H0B(0.5)
 C0AA(0.5) H0AA(0.5) H0AB(0.5) O0(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) C01S(0.5)
 H15(0.5) HV(0.5) O00N(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) C3AA(0.5) H3AA(0.5)
 H3AB(0.5)
5.a Ternary CH refined with riding coordinates:
 C00O(H00O), C00U(H00U), C010(H010), C016(H016)
5.b Secondary CH2 refined with riding coordinates:
 C00P(H00D,H00E), C00Q(H00F,H00I), C00S(H00J,H00K), C00V(H00M,H00P), C00W(H00Q,
 H00R), C00Y(H00S,H00V), C011(H3,H), C012(H4,HA), C013(H5,HB), C014(H6,HC),
 C015(H7,HD), C01A(H8,HE), C01C(H9,HF), C01D(H10,HG), C01F(H11,HH), C01H(H12,
 HI), C01I(H13,HJ), C01R(H14,HU), C0(H0A,H0B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB),
  C01S(H15,HV), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB)
5.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00L(H00L), C00N(H00N), C00T(H00T), C00X(H00X)
5.d Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00C), C017(H01A,H01B,H01C), C018(H01D,H01E,H01F), C019(H01G,
 H01H,H01I), C01B(H01J,H01K,H01L), C01E(H01M,H01N,H01O), C01G(H01P,H01Q,H01R),
 C01J(H01S,H01T,H01U), C01K(H01V,H01W,H01X), C01L(H01Y,HK,HL), C01M(H01Z,HM,HN),
  C01N(H01,HO,HP), C01O(H1,HQ,HR), C01P(H2,HS,HT)
;
_shelx_res_checksum              63291
_shelx_hkl_checksum              96600
_olex2_submission_special_instructions 'No special instructions were received'