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Doubly pyrazolate-bridged dinuclear complexes of a highly constrained bis-terdentate ligand: Observation of a [high spin-low spin] state for [Fe (PMAP)][SbF] '2.25(CHO) (PMAP = 3,5-bis{[ N -(2-pyridylmethyl)amino]-methyl}-1 H -pyrazolate)

Inorganic Chemistry, ISSN: 0020-1669, Vol: 49, Issue: 10, Page: 4560-4569
2010
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The bis-terdentate pyrazole-based ligand 3,5-bis{[N-(2-pyridylmethyl)amino] methyl}-1H-pyrazole (PMAPH) was synthesized from 3,5-(1H)-pyrazoledicarbaldehyde and 2 equiv of 2-(aminomethyl)pyridine, using sodium borohydride to reduce the imine intermediate. A family of dinuclear complexes [M(PMAP)](X) was prepared by 2:2:2 reactions of MX/PMAPH/base, where M = Zn and X = BF ; M = Cu and X = ClO, BF, OAc, NO; M = Ni, Fe and X = ClO, BF; M = Fe and X = SbF . Single crystal X-ray structure determinations on four complexes: [Fe(PMAP)](BF) '2MeCN, [Ni(PMAP)](ClO )'2MeCN, [Cu(PMAP) ](BF)'2MeCN, and [Zn(PMAP)](BF)'2MeCN confirmed a dinuclear doubly pyrazolate-bridged structure for each. The two metal centers in these complexes have similar N distorted octahedral coordination spheres, with all donors provided by the two deprotonated PMAP ligands. Magnetic measurements reveal intra-dinuclear antiferromagnetic interactions for both the M = Cu and Ni [M (PMAP)](BF) complexes, with J/k = -252(2) K and J/k = -24.7(2) K (H = -2JS S), respectively. Interestingly magnetic measurements show that the complex [Fe(PMAP)](SbF )'2.25(CHO) is in a mixed high spin (HS)-low spin (LS) spin state, [HS-LS], from 300 to 1.8 K, with no sign of spin crossover to a fully low spin form [LS-LS] even at 1.8 K. © 2010 American Chemical Society.

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