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无水YCl3 与二倍量的ArONa(ArO =2 ,6 二叔丁基 4 甲基酚基 )在四氢呋喃 (THF)中反应 ,经甲苯溶液重结晶 ,高产率地合成了二芳氧基稀土氯化物 (ArO) 2 YCl(THF) 2 ·MePh。产物经元素分析和核磁共振表征 ,并测定了其晶体结构。配合物属正方晶系 ,I4( 1) /acd空间群 ,晶胞参数为a =1.8913( 1)nm ,b =1.8913( 1)nm ,c =5 .2 2 39( 1)nm ,V =18.6 86 ( 1)nm3 ,Z =16 ,Dc=1.137mg·m- 3 ,μ =1.342mm- 1 (MoKα) ,F( 0 0 0 ) =6 848,R =0 .0 46 9,Rw=0 .112 2。中心金属钇原子与二个芳氧基中的氧原子、一个氯原子和两个THF分子中的氧原子配位 ,形成一个五配位的扭曲的三角双锥几何构型。Y O(Ar)和Y Cl的键长分别为 0 .2 10 1( 3)和 0 .2 5 17( 6 )nm。
The reaction between anhydrous YCl3 and twice the amount of ArONa (ArO = 2, 6 di-tert-butyl 4-methylphenol) in tetrahydrofuran (THF) resulted in the synthesis of diaryloxy rare earth chloride (ArO) 2 YCl (THF) 2 · MePh. The product was characterized by elemental analysis and 1H NMR and its crystal structure was determined. The complexes belong to the tetragonal system, the space group I4 (1) / acd has a = 1.8913 (1) nm, b = 1.8913 (1) nm and c = 5.2229 18.6 86 (1) nm3, Z = 16, Dc = 1.137 mg · m -3, μ = 1.342 mm -1 (MoKα), F (0 0 0) = 6 848, R = 0 .0 46 9, Rw = 0 .112 2. The central metal yttrium atoms coordinate with the oxygen atoms of the two aryloxy groups, one of the chlorine atoms and the oxygen atoms of the two THF molecules to form a five-coordinate distorted triangular bipyramid geometry. The bond lengths of Y O (Ar) and Y Cl are 0.2121 (3) and 0.525 (6) nm, respectively.