Metal-organic frameworks (MOFs) are crystalline materials that are composed of an infinite array of metal nodes (single ions or clusters) linked to one another by polyfunctional organic compounds. Because of their extraordinary surface areas and high degree of control over the physical and chemical properties, these materials have received much attention in the recent literature for industrial applications, such as gas storage. As the applications of MOFs are significant, the underlying concepts for their design and synthesis may be used in the upper-level undergraduate laboratory as a vehicle for promoting student understanding of a wide variety of chemical concepts. These include targeted synthesis, crystallography, and adsorption theory of gases. This laboratory experiment involves the synthesis and full characterization of three MOFs that are derived from inexpensive materials, followed by surface area calculations, and in the case of one material, postsynthetic modification. Owing to the high focus on solid-state characterization, we believe this course will also provide students with a foundation in characterization methods they would not normally encounter in a typical inorganic chemistry laboratory course. (Contains 2 figures and 1 scheme.)