Abstract
Reaction of 2,2′-bipyridyl (bipy) under various conditions with NbX5(X = F, Cl, or Br), TaX5(X = Cl or Br), and niobium oxide trichloride gives different types of mixed ligand complexes. Solutions of metal pentahalides and niobium oxide trichloride in benzene under anhydrous conditions gave crystalline compounds of general formula MX5(bipy) and NbOCl3(bipy). Solutions of metal pentachlorides in ether under anhydrous conditions gave crystalline complexes of formula Nb2OCl8(bipy)2 and Ta4OCl18(bipy)4. Solutions of niobium pentachloride in alcohols, containing a small, controlled amount of water gave stable crystalline compounds of formula NbOCl2(OR)(bipy). Electrolytically reduced solutions of niobium pentachloride and bipyridyl in alcohol gave crystalline paramagnetic complexes of formula Nb2Cl5(OR)3(bipy)2. The compounds were characterized by analysis, X-ray powder photographs, i.r. spectra, and magnetic susceptibility measurements.