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The crystal structure of the low-temperature form of (D 5 O 2 )[SbCl 6 ] has been investigated using X-ray and neutron diffraction on powder samples and compared with the high-temperature phase. At 40 K in space group  C 2/ c  the lattice parameters are  a  = 11.938(1),  b  = 6.8968(4),  c  = 12.996(1) Å,  β  = 115.165(6)° in agreement with  Z  = 4. Although the phase transition corresponds to a 1 st  order process the similarity between high- and low-temperature form is remarkable.

The phase transition to the low-temperature form of (D 5 O 2 )[SbCl 6 ] and determination of the deuterium positions