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Formation of Hexacarbonylmanganese(I) Salts, [Mn(CO)6]+X-, in Anhydrous HF

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journal contribution
posted on 20.08.2007, 00:00 by Jens Geier, Helge Willner, Christian W. Lehmann, Friedhelm Aubke
A convenient one-step synthesis for [Mn(CO)6]+ salts has been developed. The method involves the one-electron oxidation of Mn2(CO)10 by protons in solutions of Lewis acids (BF3, (CF3)3BCO) and anhydrous HF. The molecular structure of [Mn(CO)6][BF4]·SO2 was determined by single-crystal X-ray diffraction. Crystal data:  orthorhombic, space group Cmc21; a = 8.7001(2) Å, b = 11.8497(3) Å, and c = 11.7437(3) Å; Z = 4; R1 = 0.0320 and wR2 = 0.1106. The structural, NMR, and vibrational spectroscopic properties of [Mn(CO)6]+ fit perfectly with those of the isoelectronic species [V(CO)6]-, Cr(CO)6, and [Fe(CO)6]2+.