Royal Society of Chemistry, New Journal of Chemistry, 11(34), p. 2458
DOI: 10.1039/b9nj00556k
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A conformationally flexible bis-pyridyl-bis-amide ligand, namely N,N 0 -bis-(3-pyridyl)-isophthalamide (L1), has been exploited to synthesize metalla-macro-tricyclic cryptands by reacting it with various Cu(II) salts having different counteranions. Out of the five coordination compounds, namely [{Cu(m-L1) 2 (H 2 O) 2 }ÁSO 4 Á2H 2 OÁX] (1a), [{Cu(m-L1)(H 2 O) 4 }ÁSO 4 Á 3H 2 O] p (1b), [{Cu(m-L1) 2 (H 2 O) 2 }ÁSiF 6 ÁCH 3 OHÁ4H 2 O] p (2), [{Cu(m-L1) 2 (m-Cl)}ÁClO 4 ] p (3) and [{Cu(m-L1) 2 (H 2 O)}Á(NO 3) 2 Á2H 2 OÁX] p (4a) (X = disordered solvents), compounds such as 1a, 2 and 3 are metallacryptands, of which 3 is the first example of a polymeric metalla-macro-tricyclic cryptand. The effect of the conformation-dependent ligating topology and hydrogen bonding backbone of ligand L1, and counteranions on the formation of metallacryptands is discussed. Interestingly, an important anion, namely SO 4 2À , has been separated by concomitantly crystallizing 1a and 1b from a complex mixture of anions, such as SO 4 2À , NO 3 À and ClO 4 À , by following an in situ crystallization technique. Magnetic interactions in 3 have been investigated as a typical example. Weak antiferromagnetic coupling is observed in 3, as expected given the topology of the networks.