Some novel ester ferrocenophanes have been synthesized by esterification of 1,1′-ferrocene-di(carbonyl chloride) with some diols under very dilute conditions and characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR. Suitable crystal of ester ferrocenophane b was obtained, and its crystal structure was determined by x-ray single-crystal diffraction.