Abstract: | Methyloxoniumhexafluorometallates – Synthesis, Spectroscopic Characterization and Crystal Structure of H3COH2+AsF6– Up to now the protonation of methanol as a hydrogen bridged dimethanolium ion [H(CH3OH)2]+ was observed by different X-ray crystal structure studies. Now the preparation of H3COH2+MF6– in super acid media HF/MF5 (M = As, Sb) is reported. The thermolabile and moisture sensitive salts are characterized by vibrational and NMR spectroscopy. H3COH2+AsF6– crystallizes in the monoclinic space group P21/m (No. 11) with a = 487.8(1), b = 714.0(2), c = 848.2(2) pm, β = 98.03°(2) with 2 formula units per unit cell. |