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Controlled generation of homoleptic versus heteroleptic AuI2M (M = NiII, ZnII) trinuclear complexes, which is achieved by a slight change in the diphosphine P^P linker of digold(i) metalloligands, [Au2(P^P)(d-pen)2]2- (L1P^P; d-pen = d-penicillaminate) and [Au2(P^P)(l-cys)2]2- (L2P^P; l-cys = l-cysteinate), is reported. The reactions of a 1 1 mixture of L1dppm and L2dppm (dppm = bis(diphenylphosphino)methane) with M = NiII, ZnII gave the homoleptic AuI2M complexes, [M(L1dppm)] and [M(L2dppm)], which co-crystallized to form [M(L1dppm)]·[M
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