Two rhodium compounds with similar structures have been investigated for their toxicity to cancer cells. Previous studies indicated they may not follow the same mechanism of toxicity because one is more toxic than the other in both HeLa (cervical cancer) and MDA-MB-231 (breast cancer) cells. Those two compounds contain a metal-metal bonded dirhodium core that is surrounded by four carboxylate ligands to form either dirhodium tetraacetate (Rh2(OAc)4) or dirhodium tetrabutyrate (Rh2(OBu)4). We proposed synthesizing new dirhodium compounds with a mixture of acetate and butyrate ligands to provide new complexes to investigate the apparent differences in toxicity mechanisms. This research project focused on synthesizing four new compounds: Rh2(OAc)3(OBu), cis-Rh2(OAc)2(OBu)2, trans-Rh2(OAc)2(OBu)2, and Rh2(OAc)(OBu)3. Each compound was synthesized, purified by high-performance liquid chromatography, and characterized by mass spectrometry along with proton and carbon nuclear magnetic resonance spectroscopies. These four compounds have now been tested in cancer cell studies, and it was determined that their toxicities are greater than Rh2(OAc)4, but still less than the toxicity of Rh2(OBu)4. Future studies can focus on the determination of the mechanism of toxicity for these compounds.