The reaction of lithiumpentaphenylcyclopentadiende (LiC₅Ph₅) with niobium pentachloride in dichloromethane or toluene produces insoluble red-orange solids whose C/H/Cl analyses are not consistent with C₅Ph₅NbCl₄. Addition of an acetonitrile solution of LiC₅Ph₅ with NbCl₅ gives C₅Ph₅NbCl₄ observed as a transient product by NMR spectroscopy, which then abstracts H from the acetonitrile solvent to give HC₅Ph₅ and presumably NbCl₄CH₂CN. Reversal of the order of addition gives the •C₅Ph₅ radical as characterized by MS and EPR spectroscopy. Attempts to prepare the trimethylsilyl derivative Me₃SiC₅Ph₅ (a less reducing cyclopentadienyl group) were unsuccessful. Reaction was observed only in tetrahydrofuran, producing only Me₃SiO(CH₂)₄C₅Ph₄(m-C₆H₄(CH₃)) characterized by ¹H, ¹³C NMR and mass spectroscopy. The trimethylsilyltetraphenylcyclopentadienyl derivative, Me₃Si(H)C₅Ph₄, was characterized by ¹H, ¹³C NMR and mass spectroscopy. This compound reacts with NbCl₅ to give HCl and ClSiMe₃ and a mixture of HC₅Ph₄NbCl₄ and Me₃SiC₅Ph₄NbCl₄. To address this problem, another precursor, trimethyltintetraphenylcyclopentadiene has been prepared and characterized by ¹H NMR. Preliminary studies indicate this tin deriviative undergoes cleaner reaction with niobiumpentachloride. Details of these studies will be presented.