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The aerial reaction of 2,2'-dihydroxyazobenzene (H 2 L) with bis(acetylacetonato)oxovanadium(IV) in methanol affords binuclear V v 2 O 3 L 2 . In the presence of KOH, KV v O 2 L.1.5H 2 O is isolated. Dilute acids convert VO 2 L. to V 2 O 3 L 2 via V v O(OH)L. The electronic and IR spectra of the complexesare described. In crystalline KVO 2 L.1.5H 2 O, the vanadium(V) atom has square pyramidal geometry. The base is formed by coordinated ONO atoma of L 2- and an oxo oxygen atom

The reaction of the tris(arylazo oximato)iron(II) anion, Fe(RL) 3 - (R=Me, Ph, p-MeC 6 H 4 ), with Cu(MeCN) 4 + in dichloromethane under air affords the trinuclear complex Cu II Fe II 2 (RL) 6 . In the presence of PPh 3 in the reaction mixture, the binuclear complex Cu I Fe II (RL) 3 (PPh 3 ) is isolated. The X-ray structures of CuFe(MeL) 3 (PPh 3 ) and CuFe 2 (PhL) 6 .2CH 2 Cl 2 are reported. In both complexes the Fe(RL) 3 - fragment acts as a facially disposed tridentate oximato-O 3 ligand

In the title families the ONO ligands are deprotonated forms of N-(2-hydroxyphenyl)salicylaldimine (H 2 amp), 2,2'-dihydroxyazobenzene (H 2 azp), N-(2-carboxyphenyl)salicylaldimine (H 2 amc), or 2-hydroxy-2'-carboxy-5-methylazobenzene (H 2 azc). The ON ligand is deprotonated 8-quinolinol (Hhq), and the NN ligands are 2,2'- bipyridine (bpy) or 1,10-phenanthroline (phen). Reaction of VO(acac) 2 with a mixture of H 2 amp and bpy or Hhq in methanol affords V IV O(amp)(bpy) or V V O(amp)(hq)