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_7718571
_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         '2(C40 H56 Co O2), C7 H8'
_chemical_formula_sum            'C87 H120 Co2 O4'
_chemical_formula_weight         1347.68
_chemical_name_common            2-Co
_chemical_name_systematic        2-Co
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 111.610(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.2316(15)
_cell_length_b                   10.9254(4)
_cell_length_c                   19.6425(8)
_cell_measurement_reflns_used    9129
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      77.400
_cell_measurement_theta_min      2.486
_cell_volume                     7627.9(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016)'
_computing_data_collection       'APEX4 (Bruker AXS, 2021)'
_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  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8-Venture with Photon-III'
_diffrn_measurement_method       '/f and /w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104099
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.668
_diffrn_reflns_theta_min         2.486
_exptl_absorpt_coefficient_mu    3.771
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1106 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.8036.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8070
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+8.0123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7518
_reflns_number_total             8070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00482a2.cif
_cod_data_source_block           2Co
_cod_depositor_comments
'Adding full bibliography for 7718569--7718574.cif.'
_cod_database_code               7718571
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C39 \\sim C37-C39A
 with sigma of 0.02
 C37-C38 \\sim C37-C38A
 with sigma of 0.02
 C37-C40 \\sim C37-C40A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39A) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C40)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Fixed Sof: H45A(0.5) H45B(0.5) H45C(0.5)
5.a Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C1(H1), C3(H3), C4(H4), C34(H34), C6(H6), C36(H36),
 C41(H41), C42(H42), C43(H43)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C28(H28A,
 H28B,H28C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C),
 C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C),
  C45(H45A,H45B,H45C), C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              3990
_shelx_hkl_checksum              90552
_olex2_submission_special_instructions 'No special instructions were received'