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_7718570
_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 Co O3'
_chemical_formula_sum            'C44 H64 Co O3'
_chemical_formula_weight         699.88
_chemical_name_common            2-Co.THF
_chemical_name_systematic        2-Co.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                109.675(2)
_cell_angle_beta                 105.668(2)
_cell_angle_gamma                98.353(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7146(8)
_cell_length_b                   13.4105(10)
_cell_length_c                   14.5881(10)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2615
_cell_measurement_theta_min      2.663
_cell_volume                     2006.0(2)
_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 0.995
_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  0.0976
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            81229
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.429
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             758
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane with a few drops of THF'
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0451P)^2^+1.6147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5644
_reflns_number_total             7381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00482a2.cif
_cod_data_source_block           2CoTHF
_cod_depositor_comments
'Adding full bibliography for 7718569--7718574.cif.'
_cod_database_code               7718570
_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.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C20(H20), C22(H22), C23(H23), C30(H30), C32(H32)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              59045
_shelx_hkl_checksum              39534
_olex2_submission_special_instructions 'No special instructions were received'