Microwave-Assisted Iodination: Synthesis of Heavily Iodinated 10-Vertex and 12-Vertex Boron Clusters

Microwave-assisted syntheses of heavily iodinated 10-vertex and 12-vertex closo boron clusters are reported. Salts of closo-B10I102-, 1-carba-closo-CHB9H4I5-, 1-carba-closo-CB11H6I6-, 1-carba-closo-CHB11I11-, and B12I122- were prepared in yields of 80% or better. All molecules were characterized by NMR and IR spectroscopy and mass spectrometry. The crystal structure of [Et4N][CHB9H4I5] was determined by single crystal X-ray diffraction. This salt crystallizes in the monoclinic P2(1)/c space group, a = 9.74427(12) angstrom, b = 20.7512(2) angstrom, c = 13.06589(17) angstrom, b = 101.2176(12)degrees, V = 2591.52(6) angstrom(3), Z = 4, and r(c) = 2.262g/cm(3).