Chem. Commun., 2025, Advance Article DOI: 10.1039/D5CC05091J, Communication Natalie J. Roper, George M. Hardy, Jack M. Wootton, Paul G. Waddell, James Wilson, Roly J. Armstrong Novel N–N atropisomeric peptide analogues were prepared via a highly diastereoselective multicomponent reaction and detailed configurational studies performed.