The reaction of [Cu(DapdoH2)2]2+ ions with [CrIIIL(MeOH)2Br]2+ ions (L = 1,4,7-trimethyl-1,4,7-triazacyclononane; DapdoH2 = 2,6-diacetylpyridine dioxime) produced in situ in methanol, yielded, in the presence of triethylamine, the complex [L2CrIII2(Dapdo)2(OH)2CuII2Br2](ClO4)21. It has been characterized on the basis of elemental analysis, IR spectroscopy and variable-temperature (2–298 K) magnetic susceptibility measurements. The molecular structure established by X-ray diffraction consists of a [CrIII2(µ-NO)4(µ-OH)2CuII2]4+-core, which can be considered as two edge-sharing triangular CrCu2-units. The variable-field variable-temperature magnetic measurements revealed a ground state of St = 2 with uncommon antiferromagnetic exchange interactions between the chromium(III) and copper(II) centers: JA = −79 ± 2 cm−1, JB = −17 ± 1.7 cm−1, where JA represents the interactions through a combination of oximate (>N–O-) and a hydroxo-bridging, while JB is the exchange through only a two-atom oximate (>N–O-) group.
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