Journal of the Chemical Society, Dalton Transactions p. 2117 - 2122 (1996)
Update date:2022-08-17
Topics:
Brooker, Sally
Kelly, Robert J.
An improved synthesis of 3,6-diformylpyridazine I has been elaborated. The macrocyclic complexes Pb2L1(ClO4)4 1 and [Pb2L2][ClO4]4 2 were prepared from this precursor, 1,3-diaminopropane and lead(II) perchlorate in 1:1:1 and 2:2:1 ratios respectively. The ability of lead(II) perchlorate to template the formation of the two macrocycle ring sizes, L1 = (2 + 2) and L2 = (4 + 4), simply by alteration of the reagent ratio is unprecedented. Transmetallation of 1 or 2 with manganese(II) perchlorate and an excess of sodium thiocyanate led to the formation of [Mn2L1(NCS)4] 3. Single-crystal X-ray analyses of 2 and 3 revealed that on transmetallation a ring contraction, (4 + 4) to (2 + 2), occurs. The two manganese(II) ions have irregular geometries and are inequivalent; one is six- whilst the other is seven-co-ordinate. Unusual single-atom > NCS bridging of the manganese ions occurs.
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