The diester was resynthesized to study its reported thermotropic biaxial nematic (N-b) phase. A slightly different synthesis route using a monoprotected biphenol was used. Al intermediates, as well as the final diester, were thoroughly characterized by high resolution NMR and in some cases elemental analysis to be certain that the product isolated had the correct structure. [GRAPHICS] Mesomorphic properties were determined by both hot-stage polarizing microscopy and DSC. An I-nematic-smectic C sequence was observed rather than the N-b and N-u phases reported earlier. X-ray analysis confirmed the presence of a nematic above a smectic C phase.