Journal of the Chemical Society, Dalton Transactions p. 4295 - 4301 (1996)
Update date:2022-08-30
Topics:
Begley, Michael J.
Hubberstey, Peter
Stroud, Jo
The 4,4′-bipyridine (4,4′-bipy) and 3,6-bis(imidazolyl)pyridazine (bimpydz) bridged dinuclear copper(II)-diethylenetriamine (dien) complexes, [{Cu(dien)}2(μ-diimine)][NO3] 4·xH2O (diimine = 4,4-bipy, x = 21; diimine = bimpydz, x = 05), [{Cu(dien)}2(μ-diimine)][BF4]4·4MeCN (diimine = 4,4-bipy 2 or bimpydz 6) and [{Cu(dien)}2(μ-bimpydz)]Cl4·4H2O 4, have been synthesised and characterised. Reaction of the tetrafluoroborates, 2 and 6, with NaNO2 yields the nitrites [{Cu(dien)}2(μ-diimine)][NO2][BF4] 3·xMeCN (diimine = 4,4-bipy, x = 03; diimine = bimpydz, x = 0.57). Neither the chloride nor the nitrates react with NaNO2. Structural analysis of complexes 5 and 7 has shown that although they are both based on the dinuclear cationic unit, [{Cu(dien)}2(μ-bimpydz)]4+, in 5 the bimpydz bridge adopts a transoid arrangement of imidazole molecules, whereas in 7 it adopts a cisoid arrangement, giving Cu ... Cu separations of 13.28 and 12.88 A, respectively. In 5, the dications are linked by two axially co-ordinated nitrate anions, one strongly bound, the other very weakly bound, to give chains with a ladder-type motif. In 7, the dications are bridged by μ-nitrito-κO:κN moieties to form a chain with helical geometry. The copper(II)-nitrite interaction is novel; the anion bridges the weakly binding axial positions of two square-pyramidal copper atoms using the nitrogen lone pair and the syn lone pair of an oxygen.
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