Boron halides as reagents in inorganic syntheses. Part IV. Preparation of tris-µ-chloro-hexabromo-triangulo-trirhenium(III)(3Re–Re) and Re3I9; halogen exchange reactions with Re3Cl9and the crystal structure of a sublimation product of tris-µ-chloro-hexabromo-triangulo-trirhenium(III)(3Re–Re)
- 1 January 1972
- journal article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 4,p. 500-503
- https://doi.org/10.1039/dt9720000500
Abstract
The interaction of an excess of boron tribromide and rhenium trichloride in the condensed phase affords the new mixed halide Re3Br6Cl3, identified by u.v. and far-i.r. spectra. Mass spectra confirm this approximate composition but do not provide a suitable method for characterising a mixed halide Re3(Br,Cl), because of redistribution equilibria; successive high temperature sublimation of Re3Br6Cl3 affords as the most volatile component a compound which progressively approximates to Re3Cl9. Repeated sublimation of the mixed halide afforded a crystal suitable for X-ray study. This was identified by a complete single-crystal X-ray study as probably Re3Br8Cl (although the study does not distinguish this from mixtures of Re3Br9Cl and Re3BrC6l3 or Re3Br7Cl2). The structure of these halides is based on the triangular Re3 systems in which terminal (preferentially) and bridging (subsequently) chloride ligands are replaced by bromide ligands. Interaction of boron tri-iodide and rhenium trichloride affords rhenium tri-iodide.Keywords
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