Abstract
The orthorhombic—monoclinic phase transition at Tc=369.4K in tetramethylphosphonium tetrabromocobaltate [P(CH3)4]2CoBr4 single crystal has been studied using a two-circle X-ray diffractometer. The temperature dependence of the lattice constants a(T), b(T) and c(T) have been measured from 295K to 435K. As the temperature decreases, a(T) shows a discontinuous increase at Tc, while both b(T) and c(T) show discontinuous decrease at Tc.