Abstract
[Mo(CN)4O(H2O)]2− reacts with hydrazine and salicylaldehyde in aqueous solution to give [Mo(CN)3O(salhy)]2− (Hsalhy = salicylaldehydehydrazone), isolated as green (Ph4P)2[Mo(CN)3O(salhy)] · 6H2O. In CHCl3, the product converts within seconds into (Ph4P)2[Mo(CN)3O(salhy)] · H2O · 2CHCl3 yielding microcrystals having a metallic golden sheen. The complexes were characterised by elemental analysis, t.g. and d.t.a., u.v.–vis. absorption, i.r., 1H-n.m.r. spectroscopy and by magnetic susceptibility measurements. The visible spectra in various solvents are dominated by the metal-to-ligand charge-transfer bands with absorption maxima linearly dependent on the Reichardt ET parameter. In halogenated alkanes, the unusual hipsochromic band shift is interpreted in terms of possibile solvent bonding to the metal centre. Cyclic voltammetry indicates that the salt undergoes reversible one electron oxidation with E1/2 = −0.473 V in DMSO versus ferrocene.
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