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DOI: 10.1039/A805388J (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1998, 3991-3996

An assembly compound [K(18-crown-6)(MeOH)2][Mn(5-Clsalen)(H2O)(MeOH)]2[Fe(CN)6]·4MeOH of isolated metal centers and conversion into a ferrimagnetic compound by desolvation [18-crown-6 = 1,4,7,10,13,16-hexaoxacyclooctadecane, 5-Clsalen = N,N[hair space]′-ethylenebis(5-chlorosalicylideneiminate)]

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Hitoshi Miyasaka, Hisashi Okawa, Akira Miyazaki and Toshiaki Enoki

Abstract

The reaction of [Mn(5-Clsalen)(H2O)]ClO4 with [K(18-crown-6)(H2O)2]3[Fe(CN)6] in methanol gave a double salt, [K(18-crown)(MeOH)2][Mn(5-Clsalen)(H2O)(MeOH)]2[Fe(CN)6]·4MeOH 1 [5-Clsalen = N,N[hair space]′-ethylenebis(5-chlorosalicylideneiminate), 18-crown-6 = 1,4,7,10,13,16-hexaoxacyclooctadecane]. Compound 1 crystallizes in the monoclinic space group C[hair space]2/c with cell dimensions of a = 29.065(5), b = 14.261(8), c = 18.443(6) Å, β = 98.83(2)°, Z = 4, V = 7553(4) Å3. The two [Mn(5-Clsalen)(H2O)(MeOH)]+ cations and the [Fe(CN)6]3– anion are hydrogen bonded, through the Mn–OH2[hair space][hair space]· · ·[hair space][hair space]NC–Fe and Mn–MeOH[hair space][hair space]· · ·[hair space][hair space]NC–Fe linkages, to form a two-dimensional network structure; the O[hair space][hair space]· · ·[hair space][hair space]N separation is 2.768(8) Å in the former linkage and 2.684(8) Å in the latter. The [K(18-crown-6)(MeOH)2]+ cations are situated between the two-dimensional layers. Compound 1 was partially desolvated in air to give [K(18-crown-6)][Mn(5-Clsalen)(H2O)]2[Fe(CN)6] 1′ which exhibited a short range magnetic interaction due to the local formation of magnetically coupled sublattices. Compound 1′ was fully desolvated by heating to 180 °C to give [K(18-crown-6)][Mn(5-Clsalen)]2[Fe(CN)6] 2 which exhibited spontaneous magnetization due to the formation of a network extended by Mn–NC–Fe linkages throughout the lattice.

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