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) Å, b = 20.7512(2) Å, c = 13.06589(17) Å, b = 101.2176(12)°, V = 2591.52(6) Å3, Z = 4, and rc = 2.262 g/cm3.