The dehydration process of the zeolite paulingite was investigated mea
suring the reduction of the cell constants directly in an in situ expe
riment on a single crystal X-ray diffractometer in a temperature range
from 293 K to 523 K. The water loss occurs in two steps with a platea
u at 393 K. The leveling off occurs after a unit cell reduction of 12%
(a = 33.6 Angstrom). Distance-least-squares simulations were performe
d to determine the most likely space group and the distortions of the
partially dehydrated framework structure. The collapsed framework has
symmetry I (4) over bar 3m and is characterized by elliptically deform
ed single eight-rings. The double-eight rings show the same distortion
as observed in dehydrated zeolite rho.