The atomically precise nature of nanoclusters has enabled their full structural characterizations and development of their catalytic properties. Characteristically, nanoclusters are mixed valent, containing both an oxidized metal shell and partially reduced metallic core. Several nanoclusters of second and third row transition metals, mainly silver and gold, have been readily synthesized due to the ease with which these metals can be reduced. First row transition metal clusters are an area of interest because of their low-cost and the abundance of the metal salt precursors, however, they are not well studied as these metals are more difficult to reduce and typically resist forming metal-metal bonds. To mitigate these issues, we attempted to use the ketimide ligand (R₂C=N^-) to synthesize iron nanoclusters. The ketimide ligand may promote metal-metal bonding and stabilize metal nanoclusters due to its exceptional π-accepting and π-donating abilities. Additionally, the tunability of the ketimide backbone may lend itself to generating a variety of nanocluster geometries. Preliminary results suggest the formation of a mixed valent iron cluster with a diphenyl ketimide, Fe₄(N=CPh₂)₆, is possible. The work presented will discuss the characterization of the Fe₄ cluster via nuclear magnetic resonance spectroscopy, infrared spectroscopy, and x-ray diffractometry, as well as the synthesis of two additional ligands, 9-fluorenyl and 2-adamantyl ketimide, and their potential use in iron nanocluster syntheses.