In this paper, we report the structure and apparent molecular weights of bis-(alpha,beta-D-glucopyranosyl)-polyisobutylene (Gluc-PIB-Gluc) aggregates in CDCl(3) by NMR spectroscopy. Analysis of DOSY (diffusion-ordered NMR spectroscopy) experiments of a solution of Gluc-PIB-Gluc showed the presence of aggregates that were corroborated with dynamic light scattering. The structure of the aggregates was also studied by correlation spectroscopy (COSY) and nuclear Overhauser effect spectroscopy (NOESY) experiments.