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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Preparations and structures of titanium(IV) complexes containing 8-hydroxyquinolinate and a Schiff-base N-(2-oxyphenyl)salicylideneiminate
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Preparations and structures of titanium(IV) complexes containing 8-hydroxyquinolinate and a Schiff-base N-(2-oxyphenyl)salicylideneiminate

机译：含8-羟基喹啉酸酯和席夫碱N-（2-氧苯基）水杨酰亚胺的钛（IV）配合物的制备和结构

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In methanol, the reaction of Ti(OiPr)4, N-(2-hydroxyphenyl)salicylideneimine (H2Sap) and 8-hydroxyquinoline (HQ) in stoichiometric ratio 1:1:x yielded Ti(Sap)2 precipitate as initial product even when x was as high as 10. However, when the reaction mixture with x = 2 was left standing for 12 h or more, a small amount of red crystalline Ti(Sap)Q(OMe) was isolated. Addition of wet acetonitrile to the reaction mixture with x = 10, small amount of another red crystalline [Ti(Sap)Q]2(μ-O) was obtained after standing for 2 days. The reaction between TiQ2(OiPr)2 and H2Sap in methanol with stoichiometric ratio of y:1 also yielded Ti(Sap)2 as initial product even for y as large as 10. 1H NMR investigation of the reaction of TiQ2(OMe)2 with H2Sap revealed that Ti(Sap)Q(OMe) was not detected initially. These experimental results can be explained based on a mechanism that includes: (i) rapid reaction of H2Sap with Ti(IV) centers to form Ti(Sap)2; (ii) equilibrium between TiQ2(OMe)2 and Ti(Sap)Q(OMe); (iii) equilibrium between Ti(Sap)Q(OR) and Ti(Sap)2; and (iv) limited solubilities of Ti(Sap)Q(OR) and Ti(Sap)2. The equilibrium constants and solubilities in the mechanism were determined by the 1H NMR spectral method. The structures of Ti(Sap)Q(OMe) and [Ti(Sap)Q]2(μ-O), consisting octahedrally coordinated Ti(IV), were determined by X-ray diffraction method.
机译：在甲醇中，化学计量比为1：1：x的Ti（OiPr）4，N-（2-羟苯基）水杨亚胺（H2Sap）和8-羟基喹啉（HQ）反应生成Ti（Sap）2作为初始产物沉淀x高达10。但是，当x = 2的反应混合物静置12小时或更长时间时，会分离出少量红色结晶Ti（Sap）Q（OMe）。将湿乙腈添加至x = 10的反应混合物中，静置2天后，获得少量的另一种红色结晶[Ti（Sap）Q] 2（μ-O）。化学计量比为y：1的甲醇中TiQ2（OiPr）2与H2Sap之间的反应也产生了Ti（Sap）2作为起始产物，即使y高达10也是如此.1H NMR研究了TiQ2（OMe）2与H2Sap显示最初未检测到Ti（Sap）Q（OMe）。这些实验结果可以基于以下机理进行解释：（i）H2Sap与Ti（IV）中心快速反应形成Ti（Sap）2; （ii）TiQ2（OMe）2和Ti（Sap）Q（OMe）之间的平衡; （iii）Ti（Sap）Q（OR）和Ti（Sap）2之间的平衡; （iv）Ti（Sap）Q（OR）和Ti（Sap）2的溶解度有限。机理中的平衡常数和溶解度通过1 H NMR光谱法确定。通过X射线衍射法确定了由八面体配位的Ti（IV）组成的Ti（Sap）Q（OMe）和[Ti（Sap）Q] 2（μ-O）的结构。

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