Abstract
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.
Acknowledgments
The authors thank Greg Dwulet, Clint Vorauer, and Hannah Midget for assistance with carborane syntheses.
Funding
This work was supported by the M. J. Murdock Charitable Trust, funds from Whitman College and the National Science Foundation (CHE-0922775).