New crystalline nanostructured inorganic–organic hybrid materials containing isotactic polystyrene (iPS) are prepared by means of hydrosilylation coupling of vinyl-terminated iPS with octakis(dimethylsilyloxy)silsesquioxane (Q8M8H). The number average molar mass of the iPS chains varies between 2000 and 6000 g mol−1. As a function of the iPS/Q8M8H ratio, using excess reagent, the formation of linear or star-shaped hybrid architectures is achieved. Via fractionation, it is possible to isolate well-defined linear hybrids containing one iPS chain and seven ethyl groups per silica core (iPS-Q8M8E7) as well as star-shaped hybrids containing up to eight iPS side chains (iPS6-8-Q8M8). These new iPS/polyhedral oligomeric silsesquioxane hybrid materials crystallize when the number average molar mass of iPS side chain exceeds 5500 g mol−1. The hydrosilylation coupling reaction and the resulting linear iPS-Q8M8E7 and star-shaped iPS6-8-Q8M8 are characterized by NMR spectroscopy, size exclusion chromatography (gel permeation chromatography), and polarized light microscopy. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013
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