Heteronuclear multidimensional NMR techniques are commonly used to study protein structure, function, and dynamics, yet they are rarely taught at the undergraduate level. Here, we describe a senior undergraduate laboratory where students collect, process, and analyze heteronuclear multidimensional NMR experiments using an unstudied Ig domain (Ig2 of human obscurin) in order to sequence-specifically assign this domain. In this way, this project-oriented laboratory tries to simulate an authentic biomolecular NMR research experience. Through the semester, students gain a more thorough understanding of both the specific technical aspects of multidimensional NMR analysis and the process by which raw data are converted into sequence-specific secondary structural information.