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The silylated hexatriynyl complex trans‐(C6F5)(p‐tol3P)2Pt(C≡C)3SiEt3 (PtC6TES) is converted in situ to PtC6H (wet n‐Bu4N+ F−, THF) and cross coupled with the diyne H(C≡C)2SiEt3 (HC4TES; CuCl/TMEDA, O2) to give PtC10TES (71 %). This sequence is repeated twice to afford PtC14TES (65 %) and then PtC18TES (27 %). An analogous series of reactions starting with PtC8TES gives PtC12TES (60 %), then PtC16...
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