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Oxidation of M(CO) 6 (M = Cr, Mo, W) with the synergistic oxidative system Ag[WCA]/0.5 I 2 yields the fully characterized metalloradical salts [M(CO) 6 ] + ˙[WCA] - (weakly coordinating anion WCA = [F-{Al(OR F ) 3 } 2 ] - , R F = C(CF 3 ) 3 ). The new metalloradical cations with M = Mo and W showcase a similar structural fluxionality as the previously reported [Cr(CO) 6 ] + ˙. Their reactivity increases from M = Cr &lt; Mo &lt; W and their syntheses allow for in-depth insights into the properties of the group 6 carbonyl triad. Furthermore, the reaction of NO + [WCA] - with neutral carbonyl complexes M(CO) 6 gives access to the heteroleptic carbonyl/nitrosyl cations [M(CO) 5 (NO)] + as salts of the WCA [Al(OR F ) 4 ] - , the first complete transition metal triad of their kind.

Completing the triad: synthesis and full characterization of homoleptic and heteroleptic carbonyl and nitrosyl complexes of the group VI metals