The datasets provided are for the 1H NMR, 13C NMR and where relevant 31P NMR spectra of Boc-L-cystine (lab book number AN-395), (Boc-CysTPP)2•2Cl (lab book number AN-519), and (CysTPP)2•2Cl•2HCl (lab book number AN-525), together with DEPT, HASQC and COSY spectra where these were used to assign the 1D spectra. The folder for each compound is labelled with the appropriate lab book number.  Each folder contains pdfs of the processed spectra, MestReNova manipulatable files (.mnova) and folders of the raw data.  The data were acquired on Bruker AVIII 400 and AVIII 500 spectrometers and can be processed using Bruker Topspin software.  The compounds were prepared by Abigail A. I. Norman as part of her PhD research in the laboratory of Professor Richard C. Hartley, University of Glasgow.