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Irradiation of the Keggin-type [PW 11 O 39 {Ru(NO)}] 4- ( Ru-NO ) polyoxometalate in CH 3 CN results in rapid NO ligand elimination with the formation of [PW 11 O 39 {Ru III (CH 3 CN)}] 4- ( Ru-CH 3 CN ). This complex offers an easy entry into the Ru-based chemistry of the {PW 11 Ru} complex. Attempts to substitute N 3  - for CH 3 CN in the presence of an NaN 3 excess lead a variety of products: (i) [PW 11 O 39 {Ru III (N 3 )}] 4- ( Ru-N 3  ); (ii) [PW 11 O 39 {Ru III (N 4 HC-CH 3 )}] 4- ( Ru-Tz ) as a click-reaction product; and (iii) [PW 11 O 39 {Ru II (N 2 )}] 5- ( Ru-N 2  ). UV-VIS, CV, and HR-ESI-MS techniques were used for the reaction monitoring and characterization of the products.

Easy Ligand Activation in the Coordination Sphere of Ru inside the [PW11O39]7– Backbone