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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Synthesis and structure of diamine bis(phenolate) complexes containing the Ti(OEt)-O-Ti(OEt) function
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Synthesis and structure of diamine bis(phenolate) complexes containing the Ti(OEt)-O-Ti(OEt) function

机译：具有Ti（OEt）-O-Ti（OEt）功能的二胺双酚盐配合物的合成与结构

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摘要

Reaction of diamine-bis(phenol) ligands containing a mixture of N-methyl and N,N'-dimethyl-N,N-bis(2-hydroxy-3,5-dimethylbenzyl)ethylenediamine, H2L1 and H2L3, with [Ti(OCHMe2)(4) in absolute ethanol under reflux without exclusion of air and moisture gives [(L-1)Ti (OEt-O-Ti(OEt)(L-1)] (1). [(L-3)Ti(OEt)-O-Ti(OEt)(L-3)] (2) forms when the remaining solution containing [(L-3)Ti(OEt)(2)] (3) (characterised by X-ray crystallography) is hydrolysed with H2O. For the N-methyl and N,N'-dimethyl ligand mixture H2L2 and H2L4, which contain tert-butyl groups on the ortho-positions of the aryl rings, [(L-2)Ti(OEt)-O-Ti(OEt)(L-2)] (4) forms much more slowly and [(L-4)Ti(OEt)(2)] (5) does not hydrolyse when H2O is added. When the N-protonated ligand N,N-bis(2-hydroxy-3-methyl-5-tert-butylbenzyl)ethylenediamine, H2L5, and H2L4, which contain tert-butyl groups on the ortho-positions of the aryl rings, [(L-2)Ti(OEt)-O-Ti(OEt)(L-2)] (4) forms much more slowly and [(L-4)Ti(OEt)(2)] (5) does not hydrolyse when H2O is added. When the N-protonated ligand N,N-bis(2-hydroxy-3-methyl-5-tert-butylbenzyl)ethylenediamine, H2L5, is used, rapid hydrolysis to two isomers of [(L-5)Ti(OEt-O-Ti(OEt)(L-5)] (6) occurs without addition of water. For N,N-bis(2-hydroxy-3,5-di-tert-butylbenzyl)ethylenediamine, H2L6, hydrolysis to [(L-6)Ti(OEt)-O-Ti(OEt)(L-6)] (7) occurs slowly when H2O is added. For pendant NMe2 ligand N,N-dimethyl-N',N'-bis(2-hydroxy-3-methyl-S-tert-butylbenzyl)ethylenedia mine, H2L7, the hydrolysis reaction readily gives [(L-7)Ti(OEt)-O-Ti(OEt)(L-7)] (8) for which an X-ray crystal structure was obtained. The ortho-tert-butyl ligand derivative H2L8 formed a complex analysing as [(L-8)Ti(OEt)-O-Ti(OEt)(L-8)) (9) which could not be studied further due to insolubility. Pendant pyridine ligand N-(2-pyridylmethyl)-N,N-bis(2'-hydroxy-3'-methyl-T-tert-butylbenzyl)amin e, H2L9, apparently forms isomers of [(L-9)Ti(OEt)-O-Ti(OEt)(L-9)] and possibly [{(L-9)Ti(O)(2)] from [(L-9)Ti(OEt)(2)] (10). The ortho-tert-butyl ligand derivative H2L10 formed [(L-10)Ti(OEt)-O-Ti(OEt)(L-10)] (11) for which an X-ray crystal structure was obtained.
机译：含有N-甲基和N，N'-二甲基-N，N-双（2-羟基-3,5-二甲基苄基）乙二胺，H2L1和H2L3的混合物的二胺-双（苯酚）配体与[Ti（在无水和回流的条件下于无水乙醇中的OCHMe2）（4）产生[（L-1）Ti（OEt-O-Ti（OEt）（L-1）]（1）。[（L-3）Ti （OEt）-O-Ti（OEt）（L-3）]（2）在含有[（L-3）Ti（OEt）（2）]（3）的剩余溶液中形成（通过X射线晶体学表征）对于N-甲基和N，N'-二甲基配体混合物H2L2和H2L4，在芳环的邻位含有叔丁基，[（L-2）Ti（OEt）-当添加H2O时，O-Ti（OEt）（L-2）]（4）的形成要慢得多，[（L-4）Ti（OEt）（2）]（5）不会水解。配体N，N-双（2-羟基-3-甲基-5-叔丁基苄基）乙二胺，H2L5和H2L4，在芳环的邻位含有叔丁基，[（L-2） Ti（OEt）-O-Ti（OEt）（L-2）]（4）的形成要慢得多，并且[（L-4）Ti（OEt）（2）]（5）不会水解e当添加H2O时。当使用N-质子化的配体N，N-双（2-羟基-3-甲基-5-叔丁基苄基）乙二胺H2L5时，可快速水解为[（L-5）Ti（OEt-O）的两个异构体-Ti（OEt）（L-5）]（6）无需加水即可生成，对于N，N-双（2-羟基-3,5-二叔丁基苄基）乙二胺H2L6水解为[（L -6）Ti（OEt）-O-Ti（OEt）（L-6）]（7）当添加H2O时发生缓慢。对于NMe2侧基配体N，N-二甲基-N'，N'-双（2-羟基-3-甲基-S-叔丁基苄基）亚乙基二mineH2L7，水解反应容易得到[（L-7）Ti（OEt）-O-Ti（OEt）（L-7）]（8）得到X射线晶体结构，邻叔丁基配体衍生物H 2 L 8形成为[（L-8）Ti（OEt）-O-Ti（OEt）（L-8））（9）的络合物。由于不溶性，无法进一步研究。悬垂吡啶配体N-（2-吡啶基甲基）-N，N-双（2'-羟基-3'-甲基-T-叔丁基苄基）氨基，H2L9，显然形成[[L-9）Ti（ OEt）-O-Ti（OEt）（L-9）]以及[[L-9）Ti（OEt）（2）]中可能的[{（L-9）Ti（O）（2）]（10） 。邻叔丁基配体衍生物H 2 L 10形成了[（L-10）Ti（OEt）-O-Ti（OEt）（L-10）]（11），得到了X射线晶体结构。

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