Defining the oxidation site in Cu(II) and Ni(II) Complexes of ligands combining amido, phenolato and pyridine donors
Wang, Guanqi; Philouze, Christian; Berthiol, Florian; Moreau, Yohann; Jarjayes, Olivier; Thomas, Fabrice; Dalton Transactions  (2025) –; doi:10.1039/D5DT02056E

data_7719891
_publ_section_title
;
 Defining the oxidation site in Cu(II) and Ni(II) Complexes of ligands
 combining amido, phenolato and pyridine donors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02056E
_journal_year                    2025
_chemical_formula_moiety         'C27 H28 N3 Ni O3, C16 H36 N, 0.5(C7 H8)'
_chemical_formula_sum            'C46.5 H68 N4 Ni O3'
_chemical_formula_weight         789.75
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2024-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec141 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2025-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                82.70(3)
_cell_angle_beta                 84.77(3)
_cell_angle_gamma                85.80(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4508(17)
_cell_length_b                   10.752(2)
_cell_length_c                   25.078(5)
_cell_measurement_reflns_used    41541
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.37
_cell_volume                     2246.4(8)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41541
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.366
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.757846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1657 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.7578.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       needle
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10196
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.8610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7210
_reflns_number_total             10196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02056e2.cif
_cod_data_source_block           sad
_cod_original_formula_sum        'C46.50 H68 N4 Ni O3'
_cod_database_code               7719891
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.829
_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
 C44-C45
 1.5 with sigma of 0.02
 C44-C49
 1.38 with sigma of 0.02
 C49-C50
 1.38 with sigma of 0.02
 C50-C44
 2.4 with sigma of 0.02
 C49-C45
 2.45 with sigma of 0.02
 C50-C48
 2.45 with sigma of 0.02
 C44-C46
 2.4 with sigma of 0.02
 C45-C47
 2.4 with sigma of 0.02
 C46-C48
 2.4 with sigma of 0.02
 C47-C49
 2.4 with sigma of 0.02
 C48-C44
 2.4 with sigma of 0.02
 C45-C46
 1.4 with sigma of 0.02
 C46-C47
 1.4 with sigma of 0.02
 C47-C48
 1.4 with sigma of 0.02
 C48-C49
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C50, C44, C49, C45, C48, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C50 \\sim C44 \\sim C49 \\sim C45 \\sim C48 \\sim C46 \\sim C47: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
5. Others
 Fixed Sof: C44(0.5) H44(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C49(0.5)
 C45(0.5) H45(0.5) C47(0.5) H47(0.5) C48(0.5) H48(0.5) C46(0.5) H46(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C40(H40A,H40B), C36(H36A,H36B), C28(H28A,H28B), C33(H33A,
 H33B), C38(H38A,H38B), C34(H34A,H34B), C37(H37A,H37B), C41(H41A,H41B),
 C42(H42A,H42B), C29(H29A,H29B), C30(H30A,H30B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C3(H3), C12(H12), C10(H10), C19(H19), C11(H11), C18(H18),
 C17(H17), C16(H16), C44(H44), C45(H45), C47(H47), C48(H48), C46(H46)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C35(H35A,H35B,
 H35C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C25(H25A,
 H25B,H25C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              3676
_shelx_hkl_checksum              34674
_olex2_submission_special_instructions 'No special instructions were received'