Hybrid peptides are prepared from a C-linked carbo-β-amino acid ester (R-β-Caa) and an α- aminoxy acid (R-Ama) derived from S-lactic acid. Extensive NMR (in CDCl3 solution), CD, and MD studies on the tetra-and hexapeptides led to identification of robust 12/10-mixed helices. The dipeptide repeat having an R-β-Caa and an R-Ama thus provides a “new motif” to realize a 12/10-mixed helix, for the first time, in oligomers containing R-Ama. To ...