3 years ago

Mo2B4O9—Connecting Borate and Metal-Cluster Chemistry

Mo2B4O9—Connecting Borate and Metal-Cluster Chemistry
Hellmut Eckert, Martin K. Schmitt, Amadeus-Samuel Tragl, Dirk Johrendt, Oliver Janka, Christopher Benndorf, Richard Weihrich, Hubert Huppertz, Marcos de Oliveira, Florian Pielnhofer, Bastian Joachim, Rainer Pöttgen
We report on the first thoroughly characterized molybdenum borate, which was synthesized in a high-pressure/high-temperature experiment at 12.3 GPa/1300 °C using a Walker-type multianvil apparatus. Mo2B4O9 incorporates tetrahedral molybdenum clusters into an anionic borate crystal structure—a structural motif that has never been observed before in the wide field of borate crystal chemistry. The six bonding molecular orbitals of the [Mo4] tetrahedron are completely filled with 12 electrons, which are fully delocalized over the four molybdenum atoms. This finding is in agreement with the results of the magnetic measurements, which confirmed the diamagnetic character of Mo2B4O9. The two four-coordinated boron sites can be differentiated in the 11B MAS-NMR spectrum because of the strongly different degrees of local distortions. Experimentally obtained IR and Raman bands were assigned to vibrational modes based on DFT calculations. Come together: In the field of borate crystal chemistry, Mo2B4O9 is the first compound incorporating transition-metal clusters into its crystal structure. The tetrahedral molybdenum clusters and the face-capping oxygen atoms form heterocubane-like [Mo4O4] units. The reduction of a reagent in a high-pressure experiment enabled the combination of two hitherto separated fields of research and revealed an approach to this novel substance class.

Publisher URL: http://onlinelibrary.wiley.com/resolve/doi

DOI: 10.1002/anie.201701891

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