C-Methylcalix(4) resorcinarene (CM4RA) molecule fabricated as a thin film using spin coating method was studied for an application as a sensing membrane for the detection of volatile organic compounds. The optical properties of the CM4RA films were elucidated using UV-vis spectroscopy. In addition surface plasmon resonance technique (SPR) was employed to characterize the thin film deposition process of the CM4RA thin film. Sensing properties and the film thickness of these calixresorcinarene spun films were determined from SPR measurement. Sensing measurement results showed a fast response and recovery times with a reversible response in the optical behaviour of thin films of this material. Our results can be concluded that thin film fabricated using CM4RA molecule is demonstrating a good candidate for room temperature vapour sensing application.