The data article refers to the paper “Synthesis of High-Vinyl Isoprene and Styrene Triblock Copolymers via Anionic Polymerization with Difunctional t-BuLi Initiator” . Data presented here include the number average molecular weight (Mn), the weight average molecular weight (Mw), and polydispersity index (PDI) (Mw/Mn) of the triblock copolymers poly(styrene)-b-poly(isoprene)-b-poly(styrene) (PS-b-PI-b-PS, SIS) and poly(isoprene)-b-poly(styrene)-b-poly(isoprene) (PI-b-PS-b-PI, ISI). Mn of SIS and ISI were in the range of 208,000 to 274,000 (g/mol) and PDI of SIS and ISI are located at 1.18 to 1.2, respectively. The triblock copolymers were further identified with 2D HSQC NMR spectrum. Different vinyl content (1,2- and 3,4-addition units) of polyisoprene domains were characterized in the data.
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