An X-ray diffraction study of a clathrate compound, (thiourea)(3)-CCl4
, was performed to elucidate the mechanism of phase transitions which
are characterized by the orientational ordering of CCl4 molecules. A d
iscontinuous change of lattice constants was observed at (39 +/- 2) K
indicating the second-order phase transition and a continuous change a
t (64 +/- 2) K, the first-order one. Below the upper transition temper
ature, the space group of the lattice changed from R3c to Cc. The lowe
r two phases belong to the same space group Cc, though the phase trans
ition occurred. The orientation of CCl4 molecules deduced from the str
uctural symmetry agrees with that proposed from the previous heat capa
city and NQR measurements.