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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Synthesis, structure and properties of mononuclear oxovanadium(V) alkoxides incorporating chelated ethane-1,2-diol and propane-1,3-diol
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Synthesis, structure and properties of mononuclear oxovanadium(V) alkoxides incorporating chelated ethane-1,2-diol and propane-1,3-diol

机译：含螯合乙烷-1，2-二醇和丙烷1，3-二醇的单核氧钒（V）醇盐的合成，结构和性能

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摘要

Dark coloured complexes of type VO(L)(Heg) and VO(L)(Hpd) have been synthesized in excellent yields by reacting bis(acetylacetonato)oxovanadium(IV) with H2L in the presence of excess ethane-1,2-diol (H(2)eg) and propane-19-diol (H(2)pd), respectively in acetone. Here L2- are the deprotonated forms of N-(1-hydroxyethyl)naphthaldimine (H2L1) and N-(1-hydroxy-2-methylpropyl)-naphthaldimine (H2L2). Heg(-) and Hpd(-) form five- and six-membered V(O,O) chelate rings, respectively. The crystal structure of VO(L-2) (Heg) is reported. The ONO-coordinating tridentate [ L-2](2-) spans meridionally and consists of two planar segments mutually popd along a C-N bond. The Heg(-) ligand forms a non-planar chelate ring in which the dimethylene bridge is in gauche conformation. The five V-O lengths are unequal, the shortest being V-O( ore) and the longest is V-O(alcoholic) which is subjected to the trans influence of the oxo oxygen atom. In the crystal lattice, the VO(L-2) (Heg) molecule forms an infinite chain helical pattern via intermolecular O O hydrogen bonding. Methylene H-1 resonances are systematically shifted to lower field compared to those of free H(2)eg and H(2)pd, the shift of the CH2OV resonances being particularly large. The complex multiplet H-1 structure in CDCl3 is a good indication of the rigidity of the chelate ring in solution. V-51 chemical shifts are found to be diagnostic of the alcohol-alkoxide chelate ring size, the shift of VO(L)(Heg) being similar to 25 ppm downfield from that of VO(L) (Hpd). Low V(V) /V(IV) reduction potentials (ca. - 0.30 V versus SCE) are indicative of the considerable VO3+ stabilization due to two alkoxide coordination. (C) 2000 Elsevier Science Ltd All rights reserved. [References: 43]
机译：在过量的乙烷-1,2-二醇存在下，通过使双（乙酰丙酮基）氧钒（IV）与H2L反应，以优异的产率合成了VO（L）（Heg）和VO（L）（Hpd）型深色配合物（H（2）eg）和丙烷19-二醇（H（2）pd），分别在丙酮中。在此，L2-为N-（1-羟乙基）萘二胺（H2L1）和N-（1-羟-2-甲基丙基）-萘二胺（H2L2）的去质子化形式。 Heg（-）和Hpd（-）分别形成五元和六元V（O，O）螯合环。报道了VO（L-2）（Heg）的晶体结构。 ONO配位的三齿形[L-2]（2-）横跨子午线，由沿着C-N键相互弹出的两个平面部分组成。 Heg（-）配体形成一个非平面的螯合环，其中二亚甲基桥为gauche构象。这五个V-O长度不相等，最短的是V-O（矿石），最长的是V-O（酒精），这是受到氧代氧原子的反式影响的。在晶格中，VO（L-2）（Heg）分子通过分子间的O O氢键形成无限链的螺旋图形。与游离H（2）eg和H（2）pd相比，亚甲基H-1共振被系统地转移到较低的磁场，CH2OV共振的移位特别大。 CDCl3中复杂的多重H-1结构很好地表明了溶液中螯合环的刚性。发现V-51的化学位移可以诊断出醇-醇盐螯合物的环大小，VO（L）（Heg）的位移与VO（L）（Hpd）的低场相差25 ppm。低的V（V）/ V（IV）还原电位（相对于SCE，大约为0.30 V）表明由于两个醇盐的配位，VO3 +具有相当的稳定性。 （C）2000 Elsevier Science Ltd保留所有权利。 [参考：43]

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