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The low-temperature structure of hemimorphite, Zn 4 Si 2 O 7 (OH) 2  · H 2 O, was investigated by neutron diffraction at 20 K using the “Time-Of-Flight” (TOF) method with a four-circle single-crystal diffractometer and a position-sensitive detector at the Intense Pulsed Neutron Source (IPNS) at the Argonne National Laboratory, IL. The reversible second-order phase transition, which had previously been determined at 98(2) K by optical measurements, was confirmed by two TOF neutron histograms acquired at 20 K and 120 K. Whereas the 20 K histogram showed superlattice reflections  hkl  with  k ,  l  =  n /2 and intensities up to 30  σ ( I ), these reflections were absent in the 120 K data set. In contrast to the room-temperature structure of hemimorphite ( Imm 2,  a  ∼ 8.37 Å,  b  ∼ 10.73 Å,  c  ∼ 5.12 Å), the additional reflections of the low-temperature structure lead to a supercell with  a  = 8.354(1) Å,  b  = 21.519(4) Å,  c  = 10.240(1) Å.

The low-temperature structure and phase transition of hemimorphite, Zn 4 Si 2 O 7 (OH) 2 · H 2 O