Titanium complexes of dialkanolamine ligands: Synthesis and structureстатья

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Дата последнего поиска статьи во внешних источниках: 18 июля 2013 г.

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[1] Titanium complexes of dialkanolamine ligands: Synthesis and structure / K. V. Zaitsev, S. S. Karlov, A. A. Selina et al. // European Journal of Inorganic Chemistry. — 2006. — no. 10. — P. 1987–1999. Synthesis of the title compounds, viz. [RN(CH2CH2O)-((CHRCR)-C-1 (RO)-R-2-O-3)]Ti(OiPr)(2) (13-15) and [RN(CH2CH2O)-(CHR1CR (RO)-R-2-O-3)](2)Ti (18-28), by the reaction of one or two equivalents of the corresponding dialkanolamines RN(CH2CH2OH)((CHRCRROH)-C-1-R-2-O-3) (1-12) with Ti(OiPr)(4) is reported. Other routes to [RN(CH2CH2O)((CHRCRRO)-C-1-R-2-O-3)](2)Ti, such as the reaction of Ti(CH2Ph)(4) with dialkanolamine and the reaction of TiCl4(THF)(2) with dialkanolamine/Et3N were also tested. Dimeric titanocane 16, [PhCH2N(CH2CH2O)(2)Ti-(OMe)(2)](2), was obtained from the reaction of one equivalent of dialkanolamine 3 with CpTi(OMe)(3). PhCH2N(CH2CH2O)(2)-Ti(OMenth)(2) (17) was prepared from the transalkoxylation reaction of 15 with two equivalents of menthol. The composition and structures of all novel compounds were established by H-1 and C-13 NNIR spectroscopy as well as elemental analysis data. The possible solution structure features of 13-28 are discussed. The single-crystal X-ray diffraction study of titanocane 16 clearly indicates a dimeric structure for this compound in the solid state. According to X-ray data, compounds [PhCH2N(CH2CH2O)(2)](2)Ti (19), [MeN(CH2CH2O)- (CH2CHPhO)]Ti-2 (20), [MeN(CH2CH2O)(CH2CPh2O)](2)Ti (23), erythro-[MeN(CH2CH2O)(CHPhCHPhO)](2)Ti (24), threo-MeN(CH2CH2O)(CHPhCHPhO)](2)Ti (25), and (MeN(CH2CH2O)[CH(CH2)(4)CHO])(2)Ti (27) possess a monomeric structure with a hexacoordinate titanium atom in the solid state. Among them complexes 19, 20, 23, 25, and 27 are characterized by a cis disposition of the nitrogen atoms in the coordination environment of the Ti atom, while nitrogen atoms in 24 occupy trans positions. (c) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006. [ DOI ]

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