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Wereport the construction of dumbbell-shaped hybrid moleculesfor programming their hierarchical supramolecular nanostructures througha synergetic self-assembly. Our first dumbbell-shaped hybrid moleculeis a POM–organic–POSS cocluster produced by covalentlycoupling a POM cluster and a POSS cluster together through an organictether. Structural analyses demonstrated a highly ordered lamellarmorphology with a 4.9 nm periodicity, indicating a strong thermodynamicforce driving a nanoscale phase separation of the POM and POSS blocks.The POM clusters were arranged in an orderly fashion within the POM-containinglayer with a 1.38 nm periodicity because of fixed shape and size ofthe cluster. This investigation provides in-depth understanding ofhow to construct hierarchical supramolecular nanostructures at a nanoscaleless than 5 nm by manipulating and controlling the topological shapeof hybrid molecules. [ABSTRACT FROM AUTHOR]