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Through a rational selection of the molecular components in the structure of the complex, SEOP complexes self\u2010assemble into ordered aggregates with two different hierarchical self\u2010assembled structures in an organic solvent mixture of dichloromethane and methanol in different volume ratios. FTIR, <jats:sup>1<\/jats:sup>H\u2005NMR, and X\u2010ray photoelectron spectroscopy were used to characterize the self\u2010assembly process and the involved driving forces. In a weakly polar solvent, SEOPs aggregated into fibers with a lamellar structure. When the solvent polarity was increased, SEOPs formed ribbonlike aggregates with a tetragonal structure. The change of the hierarchical self\u2010assembled structure was deduced in regard to the arrangement of alkyl chains, electrostatic interactions, and hydrogen bonding between the pyridyl groups and terminal oxygen atoms of the polyoxometalates. 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