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The reactions of the pentamethylcyclopentadienyl halfsandwich nitrosyl complexes Cp*Cr(NO) 2 I and Cp*M(NO)I 2  (M = Mo, W) with either methanolic ammonium polysulfide solutions or hydrogen selenide solutions (generated by hydrolysis of Al 2 Se 3 ) can be used to prepare cyc/o-pentachalcogenido compounds such as Cp*M(NO)(S 5 ) (M = Cr (la), Mo (2a), W (3a)) and Cp*M(NO)(Se 5 ) (M = Cr (lb), W (3b)). The chromium complex Cp*Cr(NO)(S 5 ) (la) is also formed in high yield by photodecarbonylation of Cp*Cr(CO) 2 NO in acetonitrile solution in the presence of excess sulfur. An X-ray structure analysis of Cp*W(NO)(S 5 ) (3 a) revealed a cyclo-S 5  chelate ligand in the chair conformation and an almost linear nitrosyl group.

Halfsandwich cyclo-Pentasulfido and cyclo-Pentaselenido Complexes, (η 5 -C 5 Me 5 )M(NO)(E 5 ) (E = S, Se; M = Cr, Mo, W)