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Replacement of carboxylate bridges in polynuclear nickel pivalates with 2-hydroxy-6-methylpyridine anions
Authors:M E Nikiforova  A A Sidorov  G G Aleksandrov  V N Ikorskii  I V Smolyaninov  A O Okhlobystin  N T Berberova  I L Eremenko
Institution:(1) N. S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 31 Leninsky prosp., 119991 Moscow, Russian Federation;(2) International Tomography Center, Siberian Branch of the Russian Academy of Sciences, 3a ul. Institutskaya, 630090 Novosibirsk, Russian Federation;(3) Astrakhan State Technical University, 16 ul. Tatishcheva, 414025 Astrakhan, Russian Federation;(4) Southern Scientific Center, Russian Academy of Sciences, 4 prosp. Chekhova, 344006 Rostov-on-Don, Russian Federation
Abstract:The reaction of 2-hydroxy-6-methylpyridine (HL, 1) with nonanuclear nickel trimethyl-acetate Ni9(OH)6(OOCCMe3)12(HOOCCMe3)4 (2) in MeCN with a ratio M: L = 1: 1 under mild conditions (20 °C, 15 min) led to degradation of the metal core to form the hexanuclear complex (HL)22-HL)2Ni63-OH)22-H2O)2(μ-OOCCMe3)8(η-OOCCMe3)2 (3). Further heating of 3 in acetonitrile at 80 °C for 4 h afforded the (HL)Ni63-OH)(μ32-L)3(μ,η2-L)(μ3-L)(μ 3-OOCCMe3)(μ-OOCCMe3)42-OOCCMe3) complex. The reaction with the use of a 2: 1 THF-EtOH mixture instead of acetonitrile at 50 °C gave the decanuclear complex Ni103-O)23-OH)4(μ-OOCCMe3)632-L)6(EtOH)6](H2O)2, which is also produced from compounds 1 and 2 in ethanol. The structures of the resulting complexes were established by X-ray diffraction. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 908–917, May, 2007.
Keywords:2-hydroxy-6-methylpyridine  nickel complexes  X-ray diffraction study
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