This work is an investigation into synthetic techniques used in the preparation of polynuclear transition metal complexes. Primarily, this study is focused on high temperature techniques. The starting material used was an oxo-centred trimer with the general formula [MIII 3O(O2CR)6(S)3](X) or [MIII2MIIO(O2CR)6(S)3]; where M is a first row transition metal, O2CR is a carboxylate, S is a coordinating solvent and X is an anion. These oxo-centred trimers were heated at varying temperatures, between 200 °C and 400 °C, to produce complexes with between six and twelve metal centres. (Abstract shortened by ProQuest.).