Copolymers of styrene and n-butyl acrylate were prepared by atom transfer radical polymerization (ATRP) using CuBr/N,N,N',N',N''-pentamethyl-diethylenetriamine as catalyst and Methyl 2-bromopropionate as initiator. The polydispersity of the copolymers is quite low (1.1-.3). C-13 {H-1} NMR spectra of these copolymers show that the methylene and methine signals of the main chain are compositional sensitive and highly overlapped. Even the distortionless enhancement by polarization transfer (DEPT) was not able to assign the complex and overlapping signals. Assignments of the various resonance signals were done with the help of heteronuclear single quantum coherence (HSQC), total correlation spectroscopy (TOCSY), and heteronuclear multiple bond correlation (HMBC) experiments. (c) 2005 Wiley Periodicals, Inc.