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Synthetic compounds play an important role in developing our understanding of nitrogenase enzymes, and over the years, a multitude of new metal-containing compounds have been created using nitrogenase as an inspiration. The techniques for handling coordination compounds in organic solvents are different than those commonly encountered in a biochemistry or molecular biology laboratory. This chapter describes the precautions that are essential for successful synthesis of air- and moisture-sensitive synthetic compounds and gives details of the synthesis of some coordinatively unsaturated iron-dinitrogen and iron-sulfide compounds of interest in nitrogenase research.