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_7135089
_publ_section_title
;
 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
'C24 H72 Fe2 N4 S4 Si8, 2(C18 H36 K N2 O6), 1.5(C6 H4 F2), 0.5[C6H4F2]'
_chemical_formula_sum            'C72 H152 F4 Fe2 K2 N8 O12 S4 Si8'
_chemical_formula_weight         1940.87
_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     iterative
_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                103.1830(10)
_cell_angle_beta                 92.8640(10)
_cell_angle_gamma                99.7640(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8028(5)
_cell_length_b                   15.3890(6)
_cell_length_c                   29.1949(12)
_cell_measurement_reflns_used    9481
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.39
_cell_volume                     5066.5(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            172857
_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         27.507
_diffrn_reflns_theta_min         2.025
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.8884.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         23252
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+7.7589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20210
_reflns_number_total             23252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05205j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7135086--7135089.cif.'
_cod_database_code               7135089
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Restrained distances
 F3-C68 \\sim F1-C61
 with sigma of 0.02
 F4-C69 \\sim F2-C62
 with sigma of 0.02
 C68-C67 \\sim C61-C66
 with sigma of 0.02
 C68-C69 \\sim C61-C62
 with sigma of 0.02
 C71-C72 \\sim C64-C65
 with sigma of 0.02
 C71-C70 \\sim C64-C63
 with sigma of 0.02
 C67-C72 \\sim C66-C65
 with sigma of 0.02
 C69-C70 \\sim C62-C63
 with sigma of 0.02
 F3-C67 \\sim F1-C66
 with sigma of 0.04
 F3-C69 \\sim F1-C62
 with sigma of 0.04
 F4-C68 \\sim F2-C61
 with sigma of 0.04
 F4-C70 \\sim F2-C63
 with sigma of 0.04
 C68-C72 \\sim C61-C65
 with sigma of 0.04
 C68-C70 \\sim C61-C63
 with sigma of 0.04
 C71-C67 \\sim C64-C66
 with sigma of 0.04
 C71-C69 \\sim C64-C62
 with sigma of 0.04
 C67-C69 \\sim C66-C62
 with sigma of 0.04
 C72-C70 \\sim C65-C63
 with sigma of 0.04
 C73-C74 \\sim C76-C77
 with sigma of 0.02
 C75-C74 \\sim C78-C77
 with sigma of 0.02
 C73-C75 \\sim C76-C78
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(C78) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C65) \\sim Ueq, : with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C65) \\sim Ueq, : with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F3) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C67) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(F3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Others
 Fixed Sof: F3(0.6667) F4(0.6667) C68(0.6667) C71(0.6667) H71(0.6667)
 C67(0.6667) H67(0.6667) C72(0.6667) H72(0.6667) C69(0.6667) C70(0.6667)
 H70(0.6667) F5(0.5) C73(0.5) F6(0.5) C75(0.5) H75(0.5) C74(0.5) F2(0.3333)
 F1(0.3333) C61(0.3333) C66(0.3333) H66(0.3333) C62(0.3333) C65(0.3333)
 H65(0.3333) C63(0.3333) H63(0.3333) C64(0.3333) H64(0.3333) C76(0.5) H76(0.5)
 C78(0.5) H78(0.5) C77(0.5) H77(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C34(H34A,H34B), C58(H58A,H58B), C33(H33A,H33B), C51(H51A,
 H51B), C59(H59A,H59B), C45(H45A,H45B), C40(H40A,H40B), C43(H43A,H43B),
 C52(H52A,H52B), C46(H46A,H46B), C36(H36A,H36B), C26(H26A,H26B), C44(H44A,H44B),
  C48(H48A,H48B), C56(H56A,H56B), C60(H60A,H60B), C53(H53A,H53B), C35(H35A,
 H35B), C57(H57A,H57B), C28(H28A,H28B), C50(H50A,H50B), C55(H55A,H55B),
 C25(H25A,H25B), C38(H38A,H38B), C27(H27A,H27B), C49(H49A,H49B), C39(H39A,H39B),
  C54(H54A,H54B), C32(H32A,H32B), C41(H41A,H41B), C37(H37A,H37B), C29(H29A,
 H29B), C42(H42A,H42B), C30(H30A,H30B), C31(H31A,H31B)
4.b Aromatic/amide H refined with riding coordinates:
 C71(H71), C67(H67), C72(H72), C70(H70), C75(H75), C66(H66), C65(H65),
 C63(H63), C64(H64), C76(H76), C78(H78), C77(H77)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C13(H13A,H13B,
 H13C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C15(H15A,
 H15B,H15C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C24(H24A,H24B,H24C), C8(H8A,H8B,
 H8C), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C22(H22A,H22B,H22C), C7(H7A,H7B,
 H7C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C18(H18A,
 H18B,H18C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C12(H12A,
 H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.3
_smtbx_masks_void_truncation_radius 1.3
_shelx_res_checksum              93975
_shelx_hkl_checksum              46202
_shelx_fab_checksum              26176
_olex2_submission_special_instructions 'No special instructions were received'