Abstract. Transmission electron microscopy on natural calcium metatitanate perovskite (dysanalyte) reveals the following twin laws in the orthorhombic (space group Pbnm) phase: reflection twins on the {110} and {112} planes, and 90 ~ rotation twins about the [001] axis (referred to as [001190o twin). Single crystals that were heattreated and quenched from above 1585 K exhibit a dramatic change in domain structure compared with the starting material and specimens quenched from T <1470 K. Mutually perpendicular {110} and [001190o twins are observed throughout the crystal, forming a cross-hatched domain texture. 1/21001] antiphase domains, which are very rarely observed in the starting material, also become dominant in the crystal. This change in domain structure is interpreted as due to a structural phase transition in perovskite at a temperature below 1585 K. From the point symmetry elements that describe the twin laws and the translational elements that relate the antiphase domains, the most likely phase near 1585 K is tetragonal with space group P4/mbm. These results are consistent with high-temperature powder X-ray diffraction study. On the other hand, density of the {112} twins is increased significantly in the crystal quenched from 1673 K. Twin domains are either bound by mutually perpendicular {110} and (001) walls, or by {112} walls with {110} twin domains within the polygonal {112} domains. Both twin density variation and domain morphology suggest that the crystal may be cubic at this temperature. Microstructure of a single crystal deformed at 1273 K and 3.5 GPa (within the orthorhombic stability field) is morphologically quite distinct from that of the heat-treated specimens. Dislocations dominate the microstructure and often interact with twin domain boundaries.