We synthesized mesostructured materials using layered perovskite K2NbO3F and C(n)TMACl (n = 12, 14, 16, 18) as starting materials. In the case of n = 16, lamellar phase at pH 9, 10.5 was obtained, while 2D-hexagonal phase at pH 3-7 was observed. This result indicates that the mesophase structure depends on the pH of the reacted solution. The d(100) of mesostructured materials increased with increasing length of the alkyl chain. This indicates that the periodicity of the mesostructure can be controlled by selection of the surfactant.