An integrated laboratory experiment applying concepts and techniques developed in organic chemistry, inorganic chemistry, and instrumental analysis is presented for use by students interested in undergraduate research. The experiment incorporates some advanced laboratory practices such as multistep organic synthesis and purification, detailed reaction mechanism, air-sensitive metalation techniques, variable-temperature NMR experiments, cyclic voltammetry, and single crystal X-ray crystallography. Subsequently, students are presented with an experience that mirrors fundamental inorganic chemistry research practices found in laboratories throughout the world.