Capstone teaching laboratory activities can serve as a crucial part of the undergraduate learning experience. With this in mind, a laboratory activity that combines synthesis and multiple characterization techniques has been developed for an upper-division, laboratory-based inorganic course. Complexes of Cu(II) and Ni(II) of the amino acid glycine are first synthesized. These complexes are then characterized using a variety of spectroscopic (IR, UV--vis, [superscript 1]H NMR) techniques to determine the coordination geometries of the metal centers and thermal (differential scanning calorimetry, thermal gravimetric analysis) techniques to determine the relative stabilities of geometrical isomers. Details of the activity, including procedure, experimental data, and pre/post-test, are provided.