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_7718569
_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         'C40 H58 O2'
_chemical_formula_sum            'C40 H58 O2'
_chemical_formula_weight         570.86
_chemical_name_common            LH2
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-12-30 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.643(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.3294(7)
_cell_length_b                   8.3314(4)
_cell_length_c                   11.9719(6)
_cell_measurement_reflns_used    3204
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      68.130
_cell_measurement_theta_min      4.987
_cell_volume                     1768.84(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS Inc, 2016)'
_computing_data_collection       'APEX4 (Bruker AXS Inc, 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc, 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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_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_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3195
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.491
_diffrn_source                   'ImS Diamond'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0784 before and 0.0595 after correction.
 
For component 2:
 wR2(int) was 0.0867 before and 0.0630 after correction.
 The Ratio of minimum to maximum transmission is 0.87.

Final HKLF 4 output contains 38791 reflections, Rint = 0.0703
 (15795 with I > 3sig(I), Rint = 0.0489)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0384P)^2^+0.6887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2695
_reflns_number_total             3195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00482a2.cif
_cod_data_source_block           LH2
_cod_depositor_comments
'Adding full bibliography for 7718569--7718574.cif.'
_cod_database_code               7718569
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6038(14)
 0.3962(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C9(H9), C3(H3)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C)
;
_shelx_res_checksum              6165
_shelx_hkl_checksum              45067
_olex2_submission_special_instructions 'No special instructions were received'