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_7718574
_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 H56 Ni O2, 0.5(C6 H14)'
_chemical_formula_sum            'C43 H63 Ni O2'
_chemical_formula_weight         670.64
_chemical_name_common            2-Ni
_chemical_name_systematic        2_Ni
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,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             2025-02-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-25 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                84.035(7)
_cell_angle_beta                 84.047(7)
_cell_angle_gamma                72.058(8)
_cell_formula_units_Z            2
_cell_length_a                   10.5754(10)
_cell_length_b                   13.2838(10)
_cell_length_c                   14.3962(12)
_cell_measurement_reflns_used    5353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.9860
_cell_measurement_theta_min      3.0760
_cell_volume                     1908.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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    'DIRDIFF 2008'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23356
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         4.407
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.76506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             730
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6630
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0897P)^2^+1.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4665
_reflns_number_total             6630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00482a2.cif
_cod_data_source_block           2ni
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718569--7718574.cif.
;
_cod_database_code               7718574
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.953
_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
 C1A-C1B = C1B-C1C = C1C-C1D = C1D-C1E = C1E-C1F
 1.52 with sigma of 0.02
 C1C-C1D
 1.5 with sigma of 0.02
 C1A-C1C = C1D-C1F
 2.53 with sigma of 0.04
 C1B-C1D = C1C-C1E
 2.54 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F
 with sigma of 0.02
 C1A-C1C \\sim C1C-C1E \\sim C1B-C1D \\sim C1D-C1F
 with sigma of 0.04
 C1A-C1C \\sim C1D-C1B
 with sigma of 0.02
 C1D-C1F \\sim C1C-C1E
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C1A, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) C1E(0.5)
 H1EA(0.5) H1EB(0.5) C1F(0.5) H1FA(0.5) H1FB(0.5) H1FC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB)
6.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C11(H11), C13(H13), C31(H31), C33(H33)
6.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1F(H1FA,H1FB,H1FC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;