Diastereoisomers, iron tricarbonyl, cholesteryl sorbate 4, (+)-isomer and 5, (-)-isomer, have been synthesized and resolved by fractional crystallization. The stereostructures of the complexes were proposed by chemical method and CD spectra. DSC and polarized microscope revealed that 5 shows enantiotropic cholesteric phase. The two isomers possess same mesophase behaviors on cooling. Thermal racemization of 5 has been observed, but it is inhibited in some extent by the cholesteryl group. Chromium tricarbonyl cholesteryl (p-methyl) benzoate 8 shows similar phase transition with 4.