A. Atzesdorfer et Kj. Range, SODIUM METAPERRHENATE, NAREO4 - HIGH-PRESSURE SYNTHESIS OF SINGLE-CRYSTALS AND STRUCTURE REFINEMENT, Zeitschrift fur Naturforschung. B, A journal of chemical sciences, 50(9), 1995, pp. 1417-1418
Single crystals of sodium metaperrhenate, NaReO4, have been obtained b
y oxidation of rhenium metal with sodium nitrate under high pressure-h
igh temperature conditions (modified Belt-type apparatus, 4 kbar, 400
degrees C, Au-capsules). The crystals are tetragonal, space group I4(1
)/a, with a = 5.3654(4). c = 11.732(2) Angstrom and Z = 4. The structu
re was refined to R = 0.026, R(w) = 0.013 for 382 unique, absorption-c
orrected reflections. The scheelite-type structure for NaReO4, propose
d by Beintema in 1937, could be confirmed. It consists of isolated ReO
4 tetrahedra (Re-O = 1.728(2) Angstrom), connected by NaO8 dodecahedra
([Na-O] = 2.582(2) Angstrom).