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In a seminal 1972 study, TESCxTES with x = 8, 12, 16, and 24 (TES = SiEt3) were presented as unisolable and thus only characterized by UV-visible spectroscopy. We find that TESC24TES is obtained from the reaction of trans-(C6F5)(p-tol3P)2Pt(C≡C)5SiEt3 and crude HC8TES under Hay oxidative cross coupling conditions. Hay oxidative homocouplings of HC4TES and crude HC8TES afford TESC8TES (83%) and TESC16TES (5%). A Cadiot-Chodkiewicz reaction of BrC4Br and HC4TES (2 equiv) yields TESC12TES (11%). All of these compounds are crystalline, and the crystal structures of TESC8TES and TESC16TES are determined. 

Reactions of trans‐(C6F5)(p‐tol3P)2Pt(C≡C)nSiEt3 (PtC2nSi; n = 5, 7, 9) and ex­cess PtCl in the presence of wet n‐Bu4N+ F– under Sonogashira‐type conditions (CuCl, base, other additives) afford the title compounds PtC10Pt, PtC14Pt, and PtC18­Pt in 42‐32% yields. A four‐fold substitution of the phosphine ligands in PtC10Pt by PEt3 affords Pt'C10Pt' (78%), and a Sonogashira reaction of Pt'C2H and Pt'Cl affords Pt'C2Pt' (68%). Certain sp chain extension reactions that lead to or employ the precursors PtC10Si, PtC12Si, PtC14Si, and PtC18Si sometimes give byproducts derived from C2 loss, and possible origins are discussed. 

A bimetallic Pd complex of a bis(pincer) with a diarylpyrazine core has been prepared. 

CuI catalyzes reactions of cis -(R 2 C(CH 2 PPh 2 ) 2 )Pt(CCCCH) 2 and cis -(R 2 C(CH 2 PPh 2 ) 2 )PtI 2 in secondary amine solvents HNR’ 2 to give the title adducts [(R 2 C(CH 2 PPh 2 ) 2 )Pt(CCCC)] 4 ·(H 2 NR’ 2 + I − ) n (R/R’/ n = Me/Et/1, Me/((CH 2 CH 2 ) 2 O) 0.5 /3, Et/Et/1, Et/CH 2 CHCH 2 /1; 92–42%). Crystal structures of these or closely related species establish folded Pt 4 cores containing ammonium cation guests, with NH/ and NCH/CC hydrogen bonding. DOSY NMR experiments show that the host/guest relationship can be maintained in solution.