| Summary: | This work is divided into seven chapters. Chapter one contains a brief introduction to the chemistry of ferrocene, selenium and tellurium, together with an outline of relevant electrochemical techniques. Chapter two introduces <SUP>77 </SUP>Se and <SUP>125</SUP> Te NMR spectroscopy, and contains a discussion of the electrochemistry and multinuclear NMR spectroscopy of diferrocenyl diselenide and diferrocenyl ditelluride. The molecular structure of the latter has been determined and is also described and related to its electrochemical behaviour. Chapter three contains the results of multinuclear NMR spectroscopic and electrochemical studies of progressive series of ferrocenyl alkyl chalcogenides and bis(ferrocenyl selenide) derivatives and discusses trends within the data. It is proposed that the <SUP>77</SUP>Se chemical shift of diferrocenyl selenide is anomalous. Chapter four contains details of the synthesis and characterisation by multinuclear spectroscopy and electrochemistry of pentamethylcyclopentadienyl ferrocenyl selenide. The molecular structure of the compound, which is the first example of a crystalline mono(pentamethylcyclopentadienyl)selenium derivative, has been determined and is described. The synthesis and characterisation of the analogous tetramethyl compound is also presented in chapter four. Chapter five contains a discussion of the reactions of diferrocenyl diselenide and diferrocenyl ditelluride with metal carbonyl complexes and includes characterisation by multinuclear NMR spectroscopy, cyclic voltammetry, and differential pulse voltammetry of some of the products. The molecular structure of the [W(SeFc)(CO)<SUB>4</SUB>]<SUB>2</SUB> has also been determined and is presented. Chapter six discusses miscellaneous reactions carried out, whilst chapter seven gives experimental details of all the work described in this thesis.
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