Diastereomeric dinickel(ii) complexes with non-innocent bis(octaazamacrocyclic) ligands: isomerization, spectroelectrochemistry, DFT calculations and use in catalytic oxidation of cyclohexane
Dobrov, Anatolie; Darvasiová, Denisa; Zalibera, Michal; Bučinský, Lukáš; Jelemenská, Ingrid; Rapta, Peter; Shova, Sergiu; Dumitrescu, Dan G.; Andrade, Marta A.; Martins, Luísa M. D. R. S.; Pombeiro, Armando J. L.; Arion, Vladimir B.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00154C

data_7709732
_publ_section_title
;
 Diastereomeric dinickel(ii) complexes with non-innocent
 bis(octaazamacrocyclic) ligands: isomerization, spectroelectrochemistry,
 DFT calculations and use in catalytic oxidation of cyclohexane
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00154C
_journal_year                    2022
_chemical_formula_moiety         'C46 H46 N16 Ni2 S4'
_chemical_formula_sum            'C46 H46 N16 Ni2 S4'
_chemical_formula_weight         1068.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.771(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6789(7)
_cell_length_b                   18.7474(12)
_cell_length_c                   11.7267(7)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.218
_cell_measurement_theta_min      2.172
_cell_volume                     2346.6(3)
_computing_cell_refinement       'Saint v8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Saint v8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8138
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.049
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0599P)^2^+12.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3291
_reflns_number_total             4143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00154c2.cif
_cod_data_source_block           mo_ad192k2_hkl4_p21n
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709732
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.960
_shelx_res_checksum              25257