The reaction between the 11-vertex rhodathiaborane [8, ) 2 -nido-8,7-RhSB 9 H 10 ] (1) and 3-pyridylacetonitrile affords the hydrorhodathiaborane [8, 8, ) 2 H-9-(3-Py-CH 2 CN)-nido-8,7-RhSB 9 H 9 ] (2) in good yield. Treatment of this cluster with ethylene leads to the formation of red, [1,1-(PPh 3 )(η 2 -C 2 H 4 )-3-(3-Py-CH 2 CN)-closo-1,2-RhSB 9 H 8 ] (3). Both 11-vertex polyhedral boron-based clusters have been characterized by multielement NMR spectroscopy. In addition, compound 3 has been

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... analyzed by single-crystal X-ray diffraction analysis, and is only the second ethylene ligated metallaheteroborane to be characterized in the solid state. The molecular structure of this cluster is based on an octadecahedron. In the crystal lattice, the individual clusters form layers supported by short edgeto-face -interactions between the phenyl rings of neighboring molecules.