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The photo-induced decarbonylation of Cp*Cr(CO) 2 NO in acetonitrile solution in the presence of excess sulfur leads to the cyclo-pentasulfido complex Cp*Cr(NO)(S 5 ) (1 a), while in the case of limited sulfur supply the binuclear bis(µ-disulfido) complex Cp* 2 Cr 2 (NO) 2 (µ-S 2 ) 2  (4a) is formed preferentially. The corresponding reaction with elemental selenium produces Cp* 2 Cr 2 (NO) 2 (µ-Se 2 ) 2  (4b), irrespective of the available amount of selenium. Photodecarbonylation of Cp*Mo(CO) 2 NO gives only the binuclear derivates Cp* 2 Mo 2 (NO) 2 (µ-E 2 ) (E = S (5a), Se (5b)) which are also obtained by treating Cp*Mo(NO)I 2  with H 2 S or H 2 Se, respectively. Nitrosyl loss predominates if the tungsten complex Cp*W(NO)I 2  is reacted with H 2 S; in an argon atmosphere the products are Cp*W(S)(S 2 )(I) (7a) and Cp* 2 W 2 (S) 2 (µ-S) 2  (8a), while in air some Cp*W(NO)(S 5 ) (3a) and the oxo compounds Cp*W(O)(S 2 )I (7c), Cp* 2 W 2 (O) 2 (µ-S) 2  (8c) and Cp* 2 W 2 (S)(O)(µ-S) 2  (8d) are formed. The analogous reaction with H 2 Se leads to Cp*W(NO)(Se 5 ) (3b), Cp* 2 W 2 (O) 2 (µ-Se) 2  (9c) and Cp* 2 W 2 (Se)(O)(µ-Se) 2  (9d), respectively. The binuclear tungsten complexes 8a,c,d and 9c,d contain a central W(µ-E) 2 W framework (E = S or Se) which is unaffected by air, while terminal sulfido and selenido ligands are quantitatively converted into the corresponding terminal oxo ligands in the presence of air in CH 2 C1 2  or THF solution. With the preparation of Cp* 2 W 2 (O) 2 (µ-E) 2  (E = S (8c) and Se (9c)), the series of dioxo complexes containing a pair of monochalcogen bridges (E = O, S, Se, Te) has become complete.

Sulfurization and Selenization of the Halfsandwich Nitrosylmetal Complexes Cp*M(CO) 2 NO (M = Cr, Mo) and Cp*M(NO)I 2 (M = Mo, W)

Sulfurization and Selenization of the Halfsandwich Nitrosylmetal Complexes CpM(CO) 2 NO (M = Cr, Mo) and CpM(NO)I 2 (M = Mo, W)