A research-style laboratory experiment for advanced undergraduate students is described, which includes the synthesis, characterization, and properties (porosity, stability, amphipathy) testing of the composite [Cu[subscript 2](BTC)[subscript 4/3](H[subscript 2]O)[subscript 2][subscript 6][HPW[subscript 12]O[subscript 40]·(C[subscript 4]H[subscript 12]N)[subscript 2]·25H[subscript 2]O (denoted as NENU-3, H[subscript 3]BTC = 1,3,5-benzenetricarboxylic acid). This experiment lets students experience the universal procedure of hydro(solvo)-thermal synthesis and get knowledge of general scientific research approaches as well as have hands-on experiences in diverse modern instrumental techniques (PXRD, IR and UV--vis spectroscopy, N[subscript 2] adsorption, and TG analysis) extensively used in chemical research. Most importantly, this laboratory experiment exposes students to explore the structure-property-application relationship in NENU-3 composite material through comparing the structure and properties of NENU-3 with those of its individual component materials (H[subscript 3]PW[subscript12]O[subscript 40] and Cu[subscript 3](BTC)[subscript 2]) and consulting the related literature about NENU-3 catalysis. This experiment is helpful for developing the scientific thinking of students in chemistry through completing the analysis and discussion about the structure-property-application relationship in POM@MOF.