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Soluble oligoarylenes based on naphthalene and anthracene, and fractions of different molecular weights have been studied by electron microscopy. For the examined samples, a definite interrelation is ascertained between microstructure and physicochemical properties, such as density, x‐ray parameters, heat of solution, electron paramagnetic resonance (EPR) spectra, and dark conductivity. The molecular‐weight distribution of oligoarylenes is shown to decisively influence the degree of packing of macromolecules and their physicochemical properties. This allows interpretation of some anomalous properties of oligoarylenes in comparison with the first members of the corresponding homologous series.

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