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From solutions of TeBr 4  in concentrated aqueous HBr red needles of the crystalline hexabromotellurous acid with the stoichiometric composition H 2 TeBr 6  · 8H 2 O (1) were isolated (space group P2 1 /n, a = 7.662(5), b = 9.796(6), c = 11.987(8) Å, β = 91.35(4)° at 259 Κ). If the HBr:TeBr 4  concentration ratio in the system TeBr 4 /HBr/H 2 O was kept low, a novel acid with formal composition HTe 3 Br 13  ·4 H 2 O (2) could be prepared (space group Cm, a = 13.501(5), b = 15.453(6), c = 9.153(3) Å, β = 138.11(2)° at 140 Κ). The X-ray structural analysis of 1 shows the acid to contain, besides regular octahedral [TeBr 6 ] 2-  ions (Te-Br: 2.671(4)-2.716(4) Å), [Η 9 Ο 4 ] +  hydroxonium ions (O ··· O: 2.48(3)-2.62(3) Å). The [H 9 O 4 ] +  units are linked through a hydrogen bond system (O ··· O: 2.80(3)-2.97(4) Å) to form a three-dimen-sional network. The formula has to be written as [H 9 O 4 ] 2 [TeBr 6 ]. 2 is the first acid in this class with a trinuclear anion. Its structural formula is [H 9 O 4 ][Te 3 Br 13 ]. As a fragment of the Te 4 Br, 6  cube the anion consists of three edge-sharing octahedra with a central triply bridging Br. The mean bond distances are 2.515 Å for terminal Te-Br, 2.944 Å for Te-μ 2 Br and 3.077 Å for Te—μ 3 Br. The Ο···Ο distances in the isolated [H 9 O 4 ] +  hydroxonium ions are 2.45(3)-2.57(2) A. Raman spectra of both acids are reported.

zeitschrift für naturforschung b

Synthese, Struktur und Eigenschaften der Hexabromotellur(IV)- und Tridekabromotritellur(IV)säure-Hydrate. Kristallstrukturen der Oxonium-Salze [H 9 O 4 ] 2 [TeBr 6 ] und [H 9 O 4 ][Te 3 Br 13 ] / Synthesis, Structure and Properties of Hexabromotellurous and Tridecabromotritellurous Acid Hydrates. Crystal Structures of the Oxonium Salts [H 9 O 4 ] 2 [TeBr 6 ] and [H 9 O 4 ][Te 3 Br 13 ]