摘要
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。
Reaction of anhydrous YCl_3 with 2 equiv. of NaOAr (ArO=2,6-di-tert-butyl-4-methylphenoxo) in THF at room temperature, then recrystallization from toluene, gave the bisaryloxo lanthanide chloride [(ArO)_2YCl(THF)_2](PhMe) in high yield. The product was characterized by elemental analysis, NMR spectra and X-ray single crystal structure determination. The crystal data are tetragonal, I4(1)/acd space group, a=1.8913(1) nm, b=1.8913(1) nm, c=5.2239(1) nm, V=18.686(1) nm 3, Z=16, D_c=1.137 mg·m -3, μ=1.342 mm -1 (Mo Kα), F(000)=6848, R=0.0469, R_w=0.1122. The central metal yttrium is coordinated by two terminal ArO groups, one chlorine atom and two THF molecules to form a five-coordinate distorted trigonal bipyramid. The Y-O(Ar) and Y-Cl distances are 0.2101(3) and 0.2517(6) nm, respectively.
出处
《中国稀土学报》
CAS
CSCD
北大核心
2002年第5期398-401,共4页
Journal of the Chinese Society of Rare Earths
基金
国家自然科学基金 ( 2 0 0 72 0 2 7)
江苏省教育厅 ( 0 1KJB15 0 0 0 1)
江苏省有机合成重点实验室资助项目