Two bis-phospholane copper(I) metallamacrocycles were selectively synthesized starting from the same two building blocks, namely, ligand 1 and [Cu(NCCH3)4]BF4. Reaction conditions (ligand:metal (L:M) ratio and dilution) can be tuned to… Click to show full abstract
Two bis-phospholane copper(I) metallamacrocycles were selectively synthesized starting from the same two building blocks, namely, ligand 1 and [Cu(NCCH3)4]BF4. Reaction conditions (ligand:metal (L:M) ratio and dilution) can be tuned to obtain either a paddle-wheel- (2, L:M = 3:2) or box-type complex (3, L:M = 8:4). Their structures were unequivocally determined by X-ray crystallography. The solution 31P{1H} NMR spectrum of complex 2 consists of a broad signal, as is common for such complexes, whereas complex 3 shows splitting of the 31P{1H} NMR signal into a pseudoquartet due to 63,65Cu-31P coupling, a rare occurrence exhibited only by highly symmetrical copper(I) phosphine complexes.
               
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