This advanced undergraduate laboratory experiment involves the synthesis and characterization of a metal−organic framework with microporous channels that are held intact via hydrogen bonding of the coordinated water molecules. The hydrothermal synthesis of Co 3 (BTC) 2 •12H 2 O (BTC = 1,3,5-benzene tricarboxylic acid) is carried out using one of four different reactors (stainless steel, microwave, polypropylene bottle, or sealed glass ampules) and the products are evaluated and compared using thermogravimetric analysis, powder X-ray diffraction, and IR spectroscopy. Powder X-ray diffraction is also used to monitor the changes in structure of the framework during the partial or complete removal of the associated water molecules, as well as after reabsorption of water.