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_7135086
_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         'C59 H105 Fe K N7 O8 Si4, 1[C4H8O], 2[C4H10O]'
_chemical_formula_sum            'C71 H133 Fe K N7 O11 Si4'
_chemical_formula_weight         1468.15
_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
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 106.419(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1150(19)
_cell_length_b                   19.364(2)
_cell_length_c                   25.348(3)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      23.221
_cell_measurement_theta_min      2.264
_cell_volume                     8528.9(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'XT  (Sheldrick, 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  0.1471
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            180471
_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         25.500
_diffrn_reflns_theta_min         1.933
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1394 before and 0.0812 after correction.
The Ratio of minimum to maximum transmission is 0.8139.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       plank
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         15869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1212P)^2^+2.3637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10160
_reflns_number_total             15869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05205j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7135086--7135089.cif.'
_cod_original_cell_volume        8528.7(16)
_cod_database_code               7135086
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C50(H50A,H50B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,
 H53B), C48(H48A,H48B), C47(H47A,H47B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C56(H56A,H56B), C55(H55A,H55B), C44(H44A,H44B), C54(H54A,H54B),
  C46(H46A,H46B), C45(H45A,H45B), C43(H43A,H43B), C42(H42A,H42B)
1.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C37(H37), C35(H35), C19(H19), C28(H28), C26(H26)
1.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C41(H41A,H41B,H41C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C9(H9A,H9B,H9C), C40(H40A,
 H40B,H40C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C22(H22A,H22B,
 H22C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C),
 C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84348
_shelx_hkl_checksum              75190
_shelx_fab_checksum              62782
_olex2_submission_special_instructions 'No special instructions were received'