The first chiral and luminescent cyclic trinuclear gold(I) complex, [{AuCH(PPhMe)(PhP)}], has been isolated with metalated phosphorus ylides (PY). This complex was initially obtained through the reaction of either mononuclear [CFSAuCH(PPhMe)(PhP)]OTf or dinuclear [CFS{AuCH(PPhMe)(PhP)}](OTf) thiolate-gold-phosphane complexes in the presence of NaH, followed by the abstraction of the thiopyridine moiety employing either AgOTf or [Cu(CHCN)]PF. Our quest for a more efficient synthesis route led to the development of a streamlined one-pot synthesis method, employing Ag(acac) as both a halogen abstractor and a base, offering a quicker and more direct path to this intriguing trimer.
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