2D [superscript 1]H NOESY NMR spectroscopy is routinely used to give information on the closeness of hydrogen atoms through space. This work is based on a 2D [superscript 1]H NOESY NMR spectrum of a 12 base-pair DNA duplex. This 6-h laboratory workshop aims to provide advanced-level chemistry students with a basic, yet solid, understanding of how the 3D structure of a double-stranded DNA sequence can be determined using 2D [superscript 1]H NOESY NMR spectroscopy and, hence, how structural perturbations induced by DNA binding agents such as platinum anticancer drugs are studied. Students are supplied with various sections of the 2D [superscript 1]H NOESY spectrum of the DNA sequence. Using these, as well as a molecular model as a visual aid and tool for measuring interproton distances, they are able to sequentially assign the structure of the DNA. (Contains 2 notes and 2 figures.)