Reactive molecular and non-molecular precursors with a significant degree of energetic instability have been successfully utilized in several nitride and oxide solvothermal reactions. Metal nitride syntheses commonly involve high-temperature thermolysis with ammonia or amines; nitride precursor methods are rare, primarily due to lack of suitable nitrogen sources. Some metal nitrides find use as structural ceramics, while others exhibit high energy light emission or cooperative magnetic properties. A variety of metal azide structures with M-N=N=N bonds have been known for many years; however, these materials are often energetically unstable and shock sensitive with highly exothermic decomposition properties. This presentation will describe our ongoing efforts to moderate and harness the inherently unstable but useful nature of metal azides as single-source precursors for metal nitride micro- and nanoparticle synthesis in superheated organic arene and alkane solvents. Systems under study include thermally metastable Group 13 nitrides and metal-rich late transition-metal nitrides, which are semiconducting or show ferromagnetism, respectively. As an extension of this reactive solvothermal synthesis strategy, recent developments with the use of inorganic peroxides as titanium dioxide precursors will also be described. These nanoparticulate titanias contain crystalline anatase phase components and are catalytically active towards the oxidative photodegradation of organic dyes.