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The proton positions in the phase 4 CaO · 3 Al 2 O 3  · 3 H 2 O (C 4 A 3 H 3 ) were determined by neutron diffraction exper iments at room temperature and 5 K. Two crystallographically distinct proton sites, 16 g  and 8 f  in space group  Abma,  were located from the evaluation of difference Fourier maps. Additionally, IR spectroscopic measurements were carried out to further characterise the observed OH groups. On the basis of this knowledge and due to topo logical considerations, we propose to write C 4 A 3 H 3  according to the  IUPAC  nomenclature for microporous mate rials as an interrupted framework host structure with the formula |Ca 8 (OH) 4 | 2  [Al 4  [4][1;4] Al 8  [4][1;3] . O 20  [2] (OH) 8  [1] ] 2h {3; 4-ring}  p  {0[4 6 6 8 ]} ( Abma ) –  -SOD . X-ray diffraction experiments in the temperature range from 28 K to 973 K give an insight into the thermal behaviour of the phase C 4 A 3 H 3 , and its topotac tic condensation to |Ca 8 O 2 |[Al 12  [4]  [1;4] O 24  [2] ] h {3; 4-ring} p  · {0[4 6 6 8 ]} ( I -43 m )- SOD  (C 4 A 3 ) + 6 H 2 O. The questioned fractional coordinates of the framework oxygens in the decomposition product C 4 A 3  ,  as described in the first structure de termination, were corrected by a structure refinement using the Rietveld method. It is shown unambiguously that |(OCa 4 ) 2 | · [Al 12 O 24 ]- SOD  has a sodalite-type structure.

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Proton positions in and thermal behaviour of the phase 4 CaO · 3 Al 2 O 3  · 3 H 2 O and its thermal decomposition to |(OCa 4 ) 2 |[Al 12 O 24 ]-SOD, determined by neutron/X-ray powder diffraction and IR spectroscopic investigations