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Reaction of [ 99 Tc(CO) 6 ]ClO 4 with alkali in aqueous solutions yields yellow 99 Tc 3 H(CO) 14 as the major product. On the other hand, [ 99 TcH(CO) 5 ] becomes the major product when the reaction with alkali is combined with the extraction into hexane. The molecular structure of 99 Tc 3 H(CO) 14 , determined by SCXRD, is composed of the 99 Tc 2 (CO) 9 fragment bound to the 99 Tc(CO) 5 fragment via the hydrogen bridge and weak metal−metal bond. This compound crystallizes in the monoclinic system, space group P2 1 /n, a = 9.6954(2) Å, b = 15.0985(3) Å, c = 14.5090(3) Å, and β = 104.925(2)°. 99 Tc 3 H-(CO) 14 was additionally characterized by IR spectroscopy. The mechanism of hydrolysis of [ 99 Tc(CO) 6 ]ClO 4 was suggested.

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