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The properties of these LCs and the resulting gels were investigated using polarized optical microscopy (POM), differential scanning calorimetry (DSC), X\u2010ray diffraction (XRD), and scanning electron microscopy (SEM). These polycatenars demonstrate the ability to self\u2010assemble into columnar LCs phases, exhibiting <jats:italic>p<\/jats:italic>4\u2005<jats:italic>mm<\/jats:italic> symmetry in their bulk states. In DMF solvent, ether compounds yield gels with notably more ordered, spherical flower\u2010like morphologies, while ester compounds produce gels that are less ordered and exhibit a nanosphere morphology. The findings indicate that the polarities of both the linkages and the solvents play a critical role in the formation of supramolecular nanostructures. 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