A simple single-step synthesis of [(Tc3H3)-Tc-99(CO)(12)] from [(TcO4)-Tc-99](-) and its x-ray crystal structure. Application to the production of no-carrier added [(Re3H3)-Re-188(CO)(12)]
Reduction of no-carrier added [(ReO4)-Re-188](-) (ng range) in thf-[NBu(4)]Cl with BH3 . thf under an atmosphere of CO yields [(ReCl3)-Re-188(CO)(3)](2-) and [Re-188(3)(mu-H)(3)(CO)(12)]; under similar conditions as with [(ReO4)-Re-188](-), the first mu-hydrido-bridged Tc-99 hydride carbonyl complex is prepared and structurally characterised.