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Most chemical processes in the industrial landscape utilize expensive, toxic metals to produce most of the products we use every day. The development of catalysts that use first-row transition metals that are both cheaper and less toxic has been increasingly explored due to both economic and environmental motivations. However, to be competitive with the current catalyst systems, careful tuning of the electronic and redox properties of first-row transition metals must be considered. For this reason, bimetallic complexes have become a popular area of study due to their steric and electronic tunability. Our lab has previously synthesized many heterobimetallic complexes utilizing a phosphinoamide ligand framework to support two disparate metal centers and studied both the fundamental properties and the reactivity of these complexes. This dissertation is focused on expanding the library of early/late heterobimetallic complexes and their fundamental properties, including redox properties and the effects of two disparate metals within a single complex. Synthetic routes to produce Nb/M and Ti/M complexes using a variety of phosphinoamide ligands are explored. Additionally, the impact of the heterobimetallic framework on the bond dissociation free energy (BDFE) of a hydroxide ligand terminally bound to a Zr/Co heterobimetallic complex will be examined.