In this study, the tryptophan derivative of ferrocene-1,1'-dicarboxylic acid self-assembles in toluene to form a supramolecular nanofibrillar network structure. The ferrocene bioconjugate based nanofibers are responsive toward oxidation/reduction and show thermo and redox reversibility. Interestingly, redox-induced reversible morphological transformations between nanofiber and spheroid were observed. The self-assembly was characterized by NMR spectroscopy, FT-IR spectroscopy, UV-vis spectroscopy, circular dichroism (CD), and transmission electron microscopy (TEM).