Abstract: | Dihydroxycarbeniumhexafluorometallates – Synthesis, Spectroscopic Characterization, and Crystal Structure of HC(OH)2+AsF6? The preparation of HC(OH)2+ MF6? (M = As, Sb) by protonation of HCOOH in the superacid systems HF/MF5 is reported. The very hydrolysable and thermolabile salts are characterized by vibrational and NMR spectroscopic methods. Under inert conditions they are stable at ?40°C for some weeks. HC(OH)2+AsF6? crystallizes in the orthorhombic space group Pbca (No. 61) with a = 965.8(1), b = 1582.20(16), c = 766.40(8) pm with eight formula units per unit cell. |