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An investigation into the thermolysis of diorganophoshides in co-ordinating Lewis base solvents has revealed the importance of not only reaction conditions such as time and temperature, but also the importance of organic groups on the precursor. Nanoparticles of Cd
3
P
2
have been synthesised using compounds such as [MeCd(PBu
t2
)]
3
in tri-n-octylphosphine oxide (TOPO) and 4-ethylpyridine at elevated temperatures. Distinct optical characteristics of quantum confinement effects are observed as the particle's dimensions decrease below the excitonic radius of 180 Å.