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Metal-organic frameworks (MOFs) constitute a new class of hybrid materials which are highly crystalline porous polymers composed metal ions and organic linkers. The exceptional porosity of MOFs make them superior to common sorbents for gas storage, and separations and highly promisimg materials for sensors, size- and shape-selective catalysis, molecular recognition and nanoscale reactors. The adding of inorganic nanoparticles in MOFs structure even widen their potential applications through a combination of properties of organic components, metal ions and nanoparticles. Herein we report a new method of interfacial self-organization of supramolecular assemblies containing double-decker tetra-15-crown-5-substituted lutetium phthalocyanine (LuL2), potassium ions and cerium oxide nanoparticles (CeO2NPs). The growth of supramolecular structure proceeds through a complexation of crown-ethers of LuL2 with potassium ions. The interface acts as a labile scaffold for supramolecular synthesis and it determines the spatial geometry of self-assembled structure by the adsorption of the components at the interface and their chemical affinity. The crystalline supramolecular structure was synthesized by ultrasonic stirring of two immiscible phases containing the mixture of ligand and potassium salt and the colloidal solution of ceria nanoparticles. After the equilibration, the liquid phase was evaporated slowly. The as-formed crystalline structures were deposited onto solid supports via dip coating. The SEM investigation of the morphology of the as-formed hybrid assemblies revealed the formation of the monocrystals which evolved into more splitting structure during the concentrating of the solution. The X-ray data suggest that crowns of the top deck of LuL2 are coordinated by the potassium ions to crown groups from bottom decks of four LuL2 molecules in next layer. The as-formed structures can potentially be used for storage and transport of various gases and liquids.