High yields of novel macropolyhedral selenaboranes are reported. Reactions of the monoanions of the syn- and anti-isomers of B18H22 with powdered selenium in THF variously give new macropolyhedral selenaboranes: 19-vertex [SeB18H19]- anion 1, 19-vertex [SeB18H21]- anion 2, 20-vertex [Se2B18H19]- anion 3, and 19-vertex [Se2B17H18]- anion 4. Single-cluster [hypho-Se2B6H9]- anion 5 and neutral arachno-Se2B7H9 6 also result. All of the macropolyhedrals 1, 2, 3, and 4 are characterized by NMR spectroscopy and mass spectrometry, and by single-crystal X-ray diffraction analyses. Anions 1 and 2 each consist of an 11-vertex subcluster joined by a common two-boron edge to a 10-vertex subcluster. Anion 3 consists of an 11-vertex subcluster joined by a common boron atom and an interboron link to an arachno-type 10-vertex subcluster. Unusually, anion 3 incorporates a hexagonal pyramidal intracluster structural motif in its 11-vertex subcluster. Anion 4 entails two arachno-type 10-vertex subclusters joined by a common boron atom, and with an additional intercluster boron-boron link. NMR data for syn-B18H22 and its mono- and dianions 7 and 8 and single-crystal X-ray diffraction results for these anions and also the monoanion 9 of anti-B18H22 are also reported. The oxaborane [μ-(8,9)-O-syn-B18H20]2- dianion 10 was serendipitously formed during the work and also characterized by a single-crystal X-ray diffraction study. Experimental NMR and structural findings are supported by DFT calculations throughout.

Departamento de Química Inorgánica ISQCH Universidad de Zaragoza CSIC C Pedro Cerbuna 12 ES 50009 Zaragoza Spain

Department of Chemistry and Biochemistry Baylor University Waco Texas 76798 7348 United States

Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Husinec Řež Czech Republic

School of Chemistry of the University of Leeds Leeds LS2 9JT United Kingdom

School of Natural and Environmental Sciences Newcastle University Newcastle upon Tyne NE1 7RU United Kingdom

Citace poskytuje Crossref.org

Experimental and Computational 77Se NMR Spectroscopic Study on Selenaborane Cluster Compounds