物理化学学报 >> 1985, Vol. 1 >> Issue (04): 335-339.doi: 10.3866/PKU.WHXB19850407

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双水杨醛缩乙二胺·氯·四氢呋喃合钛(Ⅲ)的合成及单晶结构研究

章士伟; 来鲁华; 邵美成; 唐有祺   

  1. 北京大学物理化学研究所
  • 收稿日期:1985-01-03 修回日期:1985-03-15 发布日期:1985-08-15

PREPARATION AND STRUCTURE OF CHLORO[N,N'-ETHYLENEBIS(SALICYLIDENEIMINATO)] TETRAHYDROFURANTITANIUM (Ⅲ)

Zhang shiwei; Lai Luhua; Shao Meicheng; Tang Youqi   

  1. Institute of Physical Chemistry, Peking University
  • Received:1985-01-03 Revised:1985-03-15 Published:1985-08-15

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摘要： TiCl_3·3THF与Salen-Na_2在THF中反应得到标题化合物。在混合溶剂中培养出单晶, 用X射线衍射法测定了结构。晶体属正交晶系, 空间群为D~(16)_(2h)—P_(bnm), a=0.7458(2), b=1.4075(6), c=1.8752(2) nm, z=4, 经最小二乘法修正最后偏离因子R=0.086, R_w=0.066。探讨了用TiCl_3·3THF直接与Salen-H_2反应只能得到四价钛的稳定配合物的原因。考察了此配合物与二氧化碳及烷基铝的作用。

Abstract: The title complex has been synthesized by reaction of TiCl_3·3THF with salenNa_2 in THF. The solution of this compound, which is very air-sensitive, is able to exist for a long time when free from air. Single crystals were obtained in ether and THF mixed solvents. Crystal structure of the complex has been determined by the direct method from diffractometer data and refined by the least-square method to final R=0.086 and R_W=0.066. The crystals are orthorhombic, space group D_(2h)~(16)-Pbnm with a=0.7458(2), b=1.4075(6), c=1.8752(2) nm, V=1.968(2) nm, z=4. Discrete molecule of Ti(salen)Cl·THF which has mirror symetry in itself sits on crystallography mirror. The co-ordinating geometry of titanium is pseudooctahedral. The reason why the reaction of TiCl·3THF with salen-H_2 only gives oxidized prnduct has been found out. The reactions between the complex and CO_2 or ALR_3 were also studied.