Isolation of [Be₃(μ-OH)₃(H₂O)₆]³⁺. Synthesis, ⁹Be NMR Spectroscopy, and Crystal Structure of [Be₃(μ-OH)₃(H₂O)₆](picrate)₃·6H₂O

Abstract

The synthesis, 9Be NMR spectrum, and molecular structure of the [Be3(μ-OH)3(H2O)6]3+ picrate salt are presented.

The Effects of Hydrolysis and Oligomerization upon the NMR Shieldings of Be+2and Al+3Species in Aqueous Solution

“…؉1 and Al(OH 2 ) 5 OH ؉2 are calculated to be deshielded by 1.97 and 8.8 ppm, respectively, vs their parent ions. Such species may be observable at very low concentration, but their quadrupole coupling constants are large and they may have large linewidths.…”

Reactions of Beryllium Halides in Liquid Ammonia: The Tetraammineberyllium Cation [Be(NH3)4]2+, its Hydrolysis Products, and the Action of Be2+ as a Fluoride‐Ion Acceptor

“…The cation is stable at pH < 3, but at higher pH values condensation reactions occur. [34] Owing to its high symmetry, its 9 Be NMR signal is sharp and BeSO 4 ·4H 2 O is used as the reference in 9 Be NMR spectroscopy. The structure of the [BeA C H T U N G T R E N N U N G (H 2 O) 4 ] 2 + cation has also been established by IR and Raman spectroscopy and single-crystal structure analyses by using X-ray and even neutron diffraction data.…”

“…[34] Its 9 Be NMR chemical shift in aqueous solution was reported to be 0.61 ppm. [34] The cation has also been found in crystals of (Ph 4 P) 2 6 ]Cl 5 [30] and [74] Upon addition of a few drops of water to BeCl 2 dissolved in liquid ammonia and after allowing the mixture to crystallize, we were able to isolate single crystals of [ (3) and to establish their composition by X-ray diffraction. For crystallographic details, see Table 1.…”

“…3 + ring is in the skew-boat conformation in the picrate salt [34] and in the boat conformation in (Ph 4 P) 2 …”

Beryllium Displacement of H+ from Strong Hydrogen Bonds

“…[15] Above pH 5.5, beryllium precipitates as a polymeric hydroxide. Beryllium in solution is typically viewed as a dication that binds hard anions such as carboxylates, with a charge/size ratio similar to that of Al…”