Monomeric M(II) (M = Fe, Co, Ni) complexes supported by bulky aryloxide ligands tethered to an arene functionality; synthesis, electrochemistry and study of the M(II)-arene interaction.
Vagiakos, Ioannis; Tsoureas, Nikolaos; Huang, Tianyin; Christodoulou, Stella; Maron, Laurent; Pickl, Thomas; Mink, János; Halter, Dominik P.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8683–8694; doi:10.1039/d5dt00482a

data_7718572
_publ_section_title
;
 Monomeric M(II) (M = Fe, Co, Ni) complexes supported by bulky aryloxide
 ligands tethered to an arene functionality; synthesis, electrochemistry
 and study of the M(II)-arene interaction.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8683
_journal_page_last               8694
_journal_paper_doi               10.1039/d5dt00482a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H64 Fe O3, 0.5(C4 H8 O)'
_chemical_formula_sum            'C46 H68 Fe O3.5'
_chemical_formula_weight         732.85
_chemical_name_common            2-Fe.THF
_chemical_name_systematic        2-Fe.THF
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_date             2024-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-30 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                108.448(3)
_cell_angle_beta                 106.081(2)
_cell_angle_gamma                98.129(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7580(11)
_cell_length_b                   13.5926(11)
_cell_length_c                   14.6117(9)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2325
_cell_measurement_theta_min      2.638
_cell_volume                     2060.3(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.16/2021-10-23 and APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 16
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0261
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47187
_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         28.295
_diffrn_reflns_theta_min         2.490
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/n-hexane'
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0425P)^2^+1.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9114
_reflns_number_total             10220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00482a2.cif
_cod_data_source_block           2FeTHF
_cod_depositor_comments
'Adding full bibliography for 7718569--7718574.cif.'
_cod_original_formula_sum        'C46 H68 Fe O3.50'
_cod_database_code               7718572
_shelx_shelxl_version_number     2016/6
_audit_contact_letter            'Date of submission: [Month] [Year].'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_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
 C1_1-C2_1 \\sim C2_1-C3_1 \\sim C3_1-C4_1
 with sigma of 0.02
 O1_1-C1_1 \\sim O1_1-C4_1
 with sigma of 0.02
 O1_1-C2_1 \\sim O1_1-C3_1
 with sigma of 0.04
 C2_1-C4_1 \\sim C1_1-C3_1
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1_1 \\sim C1_1 \\sim C2_1 \\sim C3_1 \\sim C4_1: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(C2_1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 O1_1, C1_1, C2_1, C3_1, C4_1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C23(H23), C24(H24), C26(H26), C27(H27), C34(H34), C36(H36)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              67976
_shelx_hkl_checksum              8320
_olex2_submission_special_instructions 'No special instructions were received'