二(四氢糠基茚)稀土氯化物的合成及晶体结构

将四氢糠基茚锂分别与无水三氯化钇和无水三氯化钆以摩尔比2;1反应,除去不溶物和溶剂后,将产物在甲苯/THF中冷冻得到晶体(C₄H₇OCH₂C₉H₆)₂LnClLn=Y(1);Ln=Gd(2)].这两种配合物都是单分子无溶剂化合物,在空气中稳定.配合物1和2的晶体结构都属于正交晶系,P2₁2₁2₁空间群,晶胞参数分别为a=1.04252(9)nm,b=1.47455(12)nm,c=1.49799(13)nm,Z=4,Dc=1.508g/cm³;a=1.03701(10)nm,b=1.47233(12)nm,c=1.51354(14)nm,Z=4,Dc=1.699g/cm³.它们的结构相似,但空间构象不同.稀土中心离子分别与两个茚中的五元环和两个氧原子及氯原子成键,形成九配位结构.

Synthesis and Crystal Structure of Bis(tetrahydrofurfurylindenyl) Lanthanide Chlorides

Lanthanocene chlorides (C 4H 7OCH 2C 9H 6) 2LnClLn=Y(1); Ln=Gd(2)] were synthesized by the reaction of tetrahydrofurfurylindenyl lithium(in situ) with corresponding anhydrous lanthanide chorides in THF. The crystal structures of these two complexes were determined by X-ray diffraction and they were unsolvated monomeric complexes. They were stable in the air for several hours. Complexes 1 and 2 belong to the same crystal system(orthorhombic) and space group(P2 12 12 1). The unit cell dimensions of complex 1 were a=1\^042 52(9) nm, b=1\^474 55(12) nm, c=1\^497 99(13) nm, Z=4, D c=1\^508 \{g/cm 3\}; The unit cell dimensions of complex 2 were a=1\^037 01(10) nm, b= 1\^472 33(12) nm, c=\{1\^513 54\}(14) nm, Z=4, D c=1\^699 g/cm 3. They have the same structure and different space configurations. The central metal atom is coordinated by two indenyl, two oxygen of the tetrahydrofurfuryl and one chlorine atom to form a distorted trigonal bipyramid.