Transition metal mediated asymmetric catalysis is one of the most active areas of today's organic chemistry. In this context, helically-chiral polymers without chirality besides the helical conformation of the backbone, that have been developed by the Reggelin group, represent a new type of ligands. This Ph. D.-thesis aimed at the synthesis of helical polymethacrylates containing sterically congested side groups to improve the enantioselectivity in catalytic reactions. Furthermore, structural analysis of oligomeric methacrylates were conducted to render a rational ligand design possible. Three 2,2’-bipyridin-substituted methacrylate monomers were synthesised, whereas an orthogonal correlation between the monomer’s quality as ligands for palladium and their appropriateness for the polymerisation was found. Hence, it was not possible to synthesise a polymer of this type suitable for asymmetric catalysis. Those monomers showing high catalytic activity did not lead to a polymer, while the successfully prepared polymer did not posess catalytical activity. Nine monomers containing phenyl-bis-(2-pyridyl)-substitution with additional steric demand within the side chains were synthesised. All of them were polymerised successfully using tritylmethacrylate as a comonomer. The palladium-complexes of these monomers were studied intensively by modern NMR-spectroscopy. The product of the palladium-catalysed allylic substitution reaction of diphenylpropenyl acetate with dimethyl malonate could be isolated in high yields and with significant enantiomeric excesses up to 62% using these copolymers as ligands. Structural analysis using NOE-spectroscopy and subsequent DG-calculation requires a complete assignement of proton-signals via scalar couplings, which is not feasible in the systems under consideration using routine methods. Therefore, one position in the monomer-structure was selectively 13C-labelled and the n,m-ADEQUATE-technology was successfully implemented and optimised for the analytical problem.