This sequence of three guided-inquiry labs is designed for a second-semester general chemistry course and challenges students to discover basic theoretical principles associated with [superscript 13]C NMR, [superscript 1]H NMR, and IR spectroscopy. Students learn to identify and explain basic concepts of magnetic resonance and vibrational spectroscopy; collect and interpret sets of [superscript 13]C NMR, [superscript 1]H NMR, and IR spectra; and correctly identify functional groups and chemical structures for a variety of simple organic compounds. Student survey data, along with in-lab observations of student interactions, lead to the conclusion that these lab experiences enhance student interest, increase communication between students, and improve their ability to explain and correct their own misconceptions. (Contains 2 tables and 3 figures.)