The flexible behaviour of a trigonal arylimido iron complex.
Gonzalez, Andres; Casnati, Alessandra; Willingshofer, Moritz; Radovic, Aleksa; Cutsail, 3rd, George E; Demeshko, Serhiy; Meyer, Franc; Werncke, C. Gunnar; Chemical communications (Cambridge, England) 61 (2025) 18440–18443; doi:10.1039/d5cc05205j

data_7135088
_publ_section_title
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 The flexible behaviour of a trigonal arylimido iron complex.
;
_journal_issue                   93
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              18440
_journal_page_last               18443
_journal_paper_doi               10.1039/d5cc05205j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C21 H48 Fe N3 Si4, C18 H36 K N2 O6, 1[C5H12]'
_chemical_formula_sum            'C44 H96 Fe K N5 O6 Si4'
_chemical_formula_weight         998.56
_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     direct
_audit_creation_date             2025-02-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-05 deposited with the CCDC.	2025-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                110.5080(10)
_cell_angle_beta                 93.3680(10)
_cell_angle_gamma                93.3290(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6019(5)
_cell_length_b                   13.1359(4)
_cell_length_c                   17.7179(7)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    111.00
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.96
_cell_volume                     2732.63(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      111.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87900
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.568
_diffrn_reflns_theta_min         2.120
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1076 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.9493.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         15244
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0328P)^2^+1.5498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13652
_reflns_number_total             15244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05205j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7135086--7135089.cif.'
_cod_database_code               7135088
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C42) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
2. Others
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C41)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C42)=Sof(H42)=Sof(C47)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C40)=Sof(C44)=Sof(C46)=Sof(H46)=Sof(N6)=Sof(H6)=1-FVAR(1)
 Sof(N3)=Sof(H3)=Sof(C13)=Sof(C14)=Sof(C18)=Sof(C17)=Sof(H17)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C36(H36A,H36B), C37(H37A,H37B), C33(H33A,H33B), C32(H32A,
 H32B), C23(H23A,H23B), C35(H35A,H35B), C24(H24A,H24B), C31(H31A,H31B),
 C34(H34A,H34B), C25(H25A,H25B), C30(H30A,H30B), C26(H26A,H26B), C38(H38A,H38B),
  C28(H28A,H28B), C27(H27A,H27B), C39(H39A,H39B), C29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C17(H17), C15(H15), C42(H42), C46(H46), N6(H6)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C),
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C10(H10A,
 H10B,H10C), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C19(H19A,
 H19B,H19C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C48(H48A,H48B,H48C),
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              45381
_shelx_hkl_checksum              67932
_shelx_fab_checksum              23112
_olex2_submission_special_instructions 'No special instructions were received'