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The complexes [NbI2(CNtBu)6]I (1), [NbI2(CNtBu)4(tBuNHC⋮CNHtBu)]I (2), and cis-[NbI(CO)2(CNR)2dppe] (R = tBu (3a), Cy (3b)), have been prepared by oxidation of [Nb(CO)6]- with iodine in the presence of isonitrile either in a direct reaction (1 and 2) or, in the case of 3, by substitution in the intermediate [NbI(CO)4dppe]. While 1 and 3 are generated in absolute THF, 2 forms in moist THF. The X-ray structure analysis of 1·THF, 2, and 3b·toluene reveals trigonal-prismatic basic structures with the iodines capping tetragonal faces. 1 and 3b exhibit interatomic C···C distances sufficiently close to enable C−C coupling. The relevance of the coupling product 2 for reductive C−C coupling mediated by low-valent niobium is discussed.

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