摘要
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The use of di-2-pyridyl ketone ((py)(2)CO)/sulfate "blend" in nickel and zinc chemistry has yielded the neutral cubane clusters [Ni-4(SO4)(2){(py)(2)(CH)O}(4)] center dot 4MeOH center dot 3H(2)O (1 center dot 4MeOH center dot 3H(2...
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The use of di-2-pyridyl ketone ((py)(2)CO)/sulfate "blend" in nickel and zinc chemistry has yielded the neutral cubane clusters [Ni-4(SO4)(2){(py)(2)(CH)O}(4)] center dot 4MeOH center dot 3H(2)O (1 center dot 4MeOH center dot 3H(2)O) and [Zn-4 (SO4)(2){(py)(2)C(OH)O}(4) (H2O)(2)] center dot 6H(2)O (2 center dot 6H(2)O). The preparation of the two complexes was achieved by the reaction of MSO4 center dot x H2O [M = Ni, x = 6 (1); M = Zn, x = 7 (2)] with (py)(2)CO and LiOH center dot H2O in MeOH/H2O (for both complexes) or MeOH/MeCN (only for 1). The structures of both compounds have been determined by single-crystal X-ray crystallography. Di-2-pyridyl ketone exists in its monoanionic gem-diol form and functions as an eta(1):eta(3):eta(1):mu(3) ligand. Both complexes have been characterized by spectroscopic techniques (IR, Raman). Thermal decomposition (TG, DTG and DTA) data for 2 are also discussed. The magnetic properties of I have been studied by variable-temperature dc magnetic susceptibility techniques. The studies indicate both ferromagnetic and antiferromagnetic coupling between the four Ni-II atoms. A three-J model was found to be adequate for describing the thermal variation of the molar magnetic susceptibility. (c) 2006 Elsevier B.V. All rights reserved.
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