Studies of 2,5;6,10;8,10-Tri-µ-hydro-nonahydro-nido-nonaborate(1–), [B9H12]–: preparation, crystal and molecular structure, nuclear magnetic resonance spectra, electrochemistry and reactions

Grant B. Jacobsen, Dominic G. Meina, John H. Morris, Colin Thomson, Steven J. Andrews, David Reed, Alan J. Welch, Donald F. Gaines

Research output: Contribution to journalArticle

Abstract

Studies of 2,5;6,10;8,10-tri-μ-hydro-nonahydro-nido-nonaborate(1-) [B9H12]- have involved new syntheses, which have led to crystals suitable for the determination of the X-ray crystal and molecular structure, through reactions of B9H13(SMe2) with [OCN]- or other bases. Crystallographic study of [N(PPh3)2] [B9H12] reveals the structure of the anion to be that of a nido-nine-vertex cage, based on the parent bicapped square antiprism with one 5-connected vertex removed. The pentagonal open face is symmetrically bridged by three (μ-H) atoms (two involving the lowest connected boron), conferring effective Cs symmetry upon the polyhedron. Crystals are monoclinic, space group P21/n, with a = 26.759(10), b = 10.340(4), c = 27.044(5) Å, β = 103.47(2)°, and Z = 8. Using 6 777 diffracted intensities recorded at 185 K on an Enraf-Nonius CAD4 diffractometer, the structure has been refined to R 0.0847, R′ 0.1216. The 11B, two-dimensional 11B(COSY), and 1H n.m.r. parameters all confirm the structural assignment and the n.m.r. spectra have been assigned unambiguously. Cyclic and a.c. voltammetry and coulometry of [B9H12]- in several solvents at Pt led to the electrochemical parameters and to an isomer-specific electrochemical synthesis of anti-[B18H21]-. Chemically, the [N(PPh3)2]+ salt of [B9H12]- reacted with HCl to give [B9H13Cl]-, whereas the [NBun4]+ salt yielded anti- B18H22; reactions with CF3CO2H gave primarily anti-[B18H21]-.

Original languageEnglish
Pages (from-to)1645-1654
Number of pages10
JournalJournal of the Chemical Society, Dalton Transactions
Issue number8
DOIs
Publication statusPublished - 1985

ASJC Scopus subject areas

  • Chemistry(all)

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