Ligand HSar contained two terminal amidophenolate units that were connected by a disulfane bridge. The ligand reacted with VOSO·5HO in the presence of EtN under air and provided a mononuclear octahedral oxidovanadium complex (1). X-ray crystal structure analysis of complex 1 revealed that the oxidation state of the V ion was V and the VO unit was coordinated to an iminosemiquinone radical anion. An isotopic signal at g = 1.998 in the X-band electron paramagnetic resonance (EPR) spectrum and the solution magnetic moment μ = 1.98 μ at 298 K also supported the composition. The formation of complex 1 preceded through the initial generation of a diamagnetic VO-iminoisemiquinone species, as established by time-dependent UV-vis-near-IR (NIR), X-band EPR, and density functional theory studies. The UV-vis-NIR spectrum of complex 1 consisted of four ligand-to-metal charge-transfer transitions in the visible region, while an intervalence ligand-to-ligand charge transfer appeared at 1162 nm. The cyclic voltammogram of the complex showed four oxidation waves and one reduction wave. Spectroelectrochemical studies at fixed potentials revealed that the oxidation and reduction processes were ligand-based.
In the presence of FeCl3 and Et3N, a ligand H4Ldtda(AP) underwent S-S bond cleavage and generated a pincer non-innocent H3LONS ligand, which formed a homoleptic, six-coordinate, low-spin Fe(iii) complex (1). The complex comprised two 2-iminobenzosemiquinone (1-) π-radicals and one thiyl π-radical.
A thermodynamically unstable amine radical and an iminosemiquinone radical-coordinated square pyramidal Cu(ii) complex are isolated and established by X-ray crystallography, magnetic and EPR measurements, and DFT calculations.
The long-range antiferromagnetic coupling impeded electron flow through hexaradical-containing tetranuclear CoIII4 complex (1), while nonradical-containing tetranuclear CoIII4 complex (2), with no paramagnetic centres, was a semiconductor and sensed NH3 efficiently...
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