21107-45-9Relevant articles and documents
An experimental solution to the missing hydrogens question surrounding the macropolyhedral 19-vertex boron hydride monoanion [B 19H22]-, a simplification of its synthesis, and its use as an intermediate in the first example of syn -B18H 22 to anti -B18H22 isomer conversion
Londesborough, Michael G. S.,Bould, Jonathan,Base, Tomas,Hnyk, Drahomir,Bakardjiev, Mario,Holub, Josef,CisaRova, Ivana,Kennedy, John D.
, p. 4092 - 4098 (2010/07/04)
The macropolyhedral [B19H22]- monoanion 1 and the dianion [B19H21]2- 2 are synthesized in consistent 86-92% yields by the reaction of [PSH]+[syn-B 18H21]- with BH3(SMe2) in 1,2-Cl2C2H4 at 72 °C. [PS is an abbreviation for Proton Sponge, 1,8-bis-(dimethylamino)naphthalene. PSH is its protonated derivative.] The molecular structures of 1 and 2 were elucidated as their [PS{BH2}]+ and [PS{BH2}]2 + salts 1a and 2a by single-crystal X-ray diffraction studies, in which all atoms were located, and supported by mass spectrometric analyses together with calculations of the cluster molecular geometries (ab ignitio and/or DFT) and of 11B chemical shifts based on GIAO-DFT shielding tensors. Acidification of dianion 2 with CF3COOH in acetonitrile, H2SO4 in dichloromethane, or aqueous HCl results in the clean formation of the monoanion [B19H22]- 1. Conversely, shaking a concentrated acetonitrile solution of 1 in 0.5 M aqueous NaOH cleanly yields the [B19H21]2- dianion 2. Reaction of a dichloromethane solution of 1 with a 36% aqueous solution of HCHO in the presence of H2SO4 quantitatively converts 1 at room temperature to a 1:1 mixture of the syn- and anti-isomers of B 18H22. This cluster dismantling process is the first example of a syn- to anti-B18H22 isomer conversion.
