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The crystal structure of bis(triethylammonium)closo-decahydrodecaborate [bis(triethylammonium) decaboranate(10)], [(C 2 H 5 ) 3 NH] 2 [B 10 H 10 ], was determined and refined (space group Pmmn, no. 59, a = 989.7, b = 1333.7, c = 903.7 pm). The compound is a versatile starting material for many substances containing the [BioHio]2- entity and its derivatives. The closo-[B 10 H 10 ] 2-  cluster is a bicapped square antiprism which is only slightly distorted. Its deviation from D 4d  symmetry is smaller than that of the B 10  cages in every other compound containing this entity that have been structurally characterised. The presence of additional (N )H ---B 3  interactions in form of multiple-centre bonds between the cations and the anions, which were postulated earlier and which should influence the cage symmetry, could not be confirmed. At 55 °C, the transition into a high temperature phase was investigated by X-ray powder diffraction. The high temperature phase crystallises in the tetragonal crystal system (a = 946.9, c = 1351.0 pm).

Crystal Structure of Bis(triethylammonium)closo-decahydrodecaborate, [(C 2 H 5 ) 3 NH] 2 [B 10 H 10 ]