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A novel procedure for ambient-pressure synthesis of pentacarbonyltechnetium halides [99TcX(CO)5] (X = Cl, Br) was developed. The procedure is based on treatment of K2[99TcX6] with a mixture of HCOOH and H2SO4 on heating. With X = I, a mixture of [99TcI(CO)5] and [99TcI(CO)4]2 was obtained. The products were characterized by elemental analysis and by 99Tc NMR and IR spectroscopy.