An integrated laboratory experiment applying concepts and techniques from organic chemistry, inorganic chemistry, and instrumental analysis is presented for use in the undergraduate curriculum. This experiment highlights the synthesis, characterization, and use of tris­(2-pyridylmethyl)­amine (TPMA) to make complexes with different metal salts. It incorporates laboratory practices such as literature searches, multistep synthesis, reaction mechanisms, NMR spectroscopy, and X-ray crystallography.