Abstract
A reinvestigation of the system (NaPo3)4/H2O has been carried out. Besides the already known tetra-hydrate and anhydrous form, a mono-hydrate in the temperature range 100–120°C exists. Single crystals were obtained by crystallization from aqueous solutions containing higher alcohols (e.g. ethyleneglycol) at ∼115°C. The crystal structure was solved by X-ray methods (orthorhombic;P212121;a=1365.4(2),b=1 347.5(3),c=629.1(3)pm;Z=4; 2774 diffractometer data;R=0.053). The cyclic anions exhibit point symmetryD2d with all terminal oxygens in eclipsed conformation. With respect to the (NaPO3)4-part of structure, mono-hydrate and anhydrous forms are isostructural; lattice parameters of the latter area=1 380.8(2),b=1 363.3(2),c=602.7(2) pm. The transition mono-hydrate to anhydrous form occurs topochemically and is reversible.
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