Collect. Czech. Chem. Commun. 1997, 62, 1310-1324

Synthesis, Spectroscopic Characterization, and Structure of closo-1,10-B10H8F22- and Related Fluorinated Derivatives of B10H102-

Sergei V. Ivanova,b, Svetlana M. Ivanovaa, Susie M. Millera, Oren P. Andersona, Nikolai T. Kuznetsovb, Konstantin A. Solntsevb and Steven H. Straussa

a Department of Chemistry, Colorado State University, Fort Collins, CO 80523, U.S.A.
b Institute of General and Inorganic Chemistry, Russian Academy of Sciences, Moscow 117907, Russia


The treatment of salts of the B10H102- anion with the commercially available N-fluoro reagent 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (F-TEDA) resulted in the formation of fluorinated derivatives of this ten-vertex borane dianion. The effects of changing the solvent, temperature, and reagent stoichiometry were studied. The derivatives 1-B10H9F2-, 2-B10H9F2-, 1,2-B10H8F22-, 1,6-B10H8F22-, 1,10-B10H8F22-, and 1,2,10-B10H7F32- were examined by a combination of 11B and 19F NMR spectroscopy and by IR spectroscopy. The salt [Ph4P]2[1,10-B10H8F2] . 3 CH2Cl2 was structurally characterized by single-crystal X-ray crystallography: C51H48B10Cl6F2P2, monoclinic, C2/c, a = 13.8134(9), b = 19.141(1), c = 21.136(1) Å, β = 91.546(1)°, Z = 4, T = -100 °C, R = 0.077.

Keywords: Decaborane; Fluorination; N-Fluoro reagents.