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

Ivanov, Sergei V.; Ivanova, Svetlana M.; Miller, Susie M.; Anderson, Oren P.; Kuznetsov, Nikolai T.; Solntsev, Konstantin A.; Strauss, Steven H.

doi:10.1135/cccc19971310

CCCC > Archive > 1997, Volume 62 > Issue 8 > p. 1310

Synthesis, Spectroscopic Characterization, and Structure of closo-1,10-B₁₀H₈F₂^2- and Related Fluorinated Derivatives of B₁₀H₁₀^2-

Sergei V. Ivanov^a,b, Svetlana M. Ivanova^a, Susie M. Miller^a, Oren P. Anderson^a, Nikolai T. Kuznetsov^b, Konstantin A. Solntsev^b and Steven H. Strauss^a

^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

Abstract

The treatment of salts of the B₁₀H₁₀^2- 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-B₁₀H₉F^2-, 2-B₁₀H₉F^2-, 1,2-B₁₀H₈F₂^2-, 1,6-B₁₀H₈F₂^2-, 1,10-B₁₀H₈F₂^2-, and 1,2,10-B₁₀H₇F₃^2- were examined by a combination of ¹¹B and ¹⁹F NMR spectroscopy and by IR spectroscopy. The salt [Ph₄P]₂[1,10-B₁₀H₈F₂] . 3 CH₂C_l2 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.

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