Metallcarbonyl‐Synthesen, XX. Einfache Methode zur Darstellung von Tc(CO) 3 ‐Komplexen: Synthese und Struktur der neuartigen Technetium(I)‐Clusterverbindung Na[Tc 3 (CO) 9 (OCH 3 ) 4 ] mit Cuban‐Struktur

Metal Carbonyl Syntheses, XX. – Simple Method for the Preparation of Tc(CO) 3 Complexes: Synthesis, Structures, and Reactivity of the Novel Cubane‐Type Cluster Na[Tc 3 (CO) 9 (OCH 3 ) 4 ] Carbonyltechnetium complexes of type LTc(CO) 3 are accessible along a simple route from Na[Tc 3 (CO) 9 (OCH 3 ) 4 ] ( 2 ) which represents a novel alkoxy complex of cubane‐type geometry (single‐crystal X‐ray diffraction study). 2 is an isolable product of the incomplete carbonylation of sodium pertechnetate ( 1 ) conducted in methanol. Under carbon monoxide pressure, 2 yields the binary metal carbonyl Tc 2 (CO) 10 ( 3 ), pentamethyl‐cyclopentadiene gives the halfsandwich complex (η 5 ‐C 5 Me 5 )Tc(CO) 3 ( 4 ), and with benzene/hydrochloric acid the ionic complex [(η 6 ‐C 6 H 6 )Tc(CO) 3 ]Cl ( 5 ) is formed.