The synthesis and the characterization of segmented liquid-crystalline [P(n)] made by interfacial polycondensation of 3-allyl-4,4＇-dihydroxybiphenyl and the acid chlorides of alpha,omega-dicarboxy-alkanes are reported. The flexible spacers contain even numbers of methylene units (n = 6-14), All polymers are enantiotropic showing a nematic phase with isotropization temperature in the range of about 95-175 degrees C. At room temperature all polymers show a mesophasic structure except for P(8) which is crystalline. Both P(12) and P(14) show a quasihexagonal phase with six chains per unit cell. (C) 2000 Elsevier Science Ltd. All rights reserved.