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Abstract:
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+.