The polymer synthesis and workup procedures were carried out as described elsewhere. Details can be found in the Supporting Information (Supporting Information Table -S8, Figure -S8). Briefly, methyl triflate was added to a dried and nitrogen-flushed Schlenk flask and dissolved in the respective amount of benzonitrile. MeOx was added, and the reaction mixture was heated to 120 °C and stirred until 1 H NMR spectroscopy revealed complete consumption of the monomer. Subsequently, the mixture was cooled to room temperature and the monomer for the second block, 2-n-butyl-2-oxazine, 2-n-butyl-2oxazoline, 2-n-pentyl-2-oxazoline and 2-n-pentyl-2-oxazine, respectively, was added. The mixture was heated to 130 °C overnight. For polymers containing PentOzi, the polymerization was heated to 150 °C until complete consumption of the monomer for the second block. The same procedure (120 °C) was repeated for the third block MeOx. After confirmation of monomer consumption by 1 H NMR, the polymerization was terminated by addition of ethyl isonipecotate or piperidine at 50 °C for 4 h. The solvent was removed under reduced pressure.