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Reduction of the Th 3+ complex Cp''3Th, 1 [Cp'' = C 5 H 3 (SiMe 3 ) 2 ], with potassium graphite in THF in the presence of 2.2.2-cryptand generates [K(2.2.2-cryptand)][Cp''3Th], 2 , a complex containing thorium in the formal +2 oxidation state. Reaction of 1 with KC 8 in the presence of 18-crown-6 generates the analogous Th 2+ compound, [K(18-crown-6)(THF) 2 ][Cp''3Th], 3 . Complexes 2 and 3 form dark green solutions in THF with ε = 23 000 M -1 cm -1 , but crystallize as dichroic dark blue/red crystals. X-ray crystallography revealed that the anions in 2 and 3 have trigonal planar coordination geometries, with 2.521 and 2.525 Å Th-(Cp'' ring centroid) distances, respectively, equivalent to the 2.520 Å distance measured in 1 . Density functional theory analysis of (Cp''3Th) 1- is consistent with a 6d 2 ground state, the first example of this transition metal electron configuration. Complex 3 reacts as a two-electron reductant with cyclooctatetraene to make Cp''2Th(C 8 H 8 ), 4 , and [K(18-crown-6)]Cp''.

chemical science

Synthesis, structure, and reactivity of crystalline molecular complexes of the {[C5H3(SiMe3)2]3Th}1− anion containing thorium in the formal +2 oxidation state