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)2YCl(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=5.2239(1) nm, V=18.686(1) nm3, Z=16, Dc=1.137 mg*m-3, μ=1.342 mm-1 (Mo Kα), F(000)=6848, R=0.0469, Rw=0.1122. 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0.2101(3) 和0.2517(6) nm.
参考文献
| [1] | Shibasaki M;Sasai H;Arai T .Asymmetric catalysis with heterobimetallic compounds[J].Angewandte Chemie International Edition,1997,36(06):1236. |
| [2] | HouZ;Tezuka H;Zhang Y et al.One-step block-copolymerization of ethylene with styrene by C5Me5/ER-ligated samarium (Ⅱ) complexes (ER = OAr SAr)[J].Macromolecules,1998,31(24):8650. |
| [3] | Mehrotra R C;Singh A;Tripathi U M .Recent advances in alkoxo and aryloxo chemistry of scandium yttrium, and lanthanoids[J].Chemical Reviews,1991,91(06):1287. |
| [4] | Yao YM.;Sun J.;Shen Q. .Synthesis and crystal structure of a monomeric aryloxo ytterbium dichloride (ArO)YbCl2(THF)(3) (ArO = 2,6-ditertbutyl-4-methylphenoxo)[J].Polyhedron: The International Journal for Inorganic and Organometallic Chemistry,1998(4):519-522. |
| [5] | HouZ;Fujita A;Yoshimura T et al.Heteroleptic lanthanide complexes with aryloxide ligands. synthesis and structural characterization of divalent and trivalent samarium aryloxide/halide and aryloxide/cyclopentadienide complexes[J].Inorganic Chemistry,1996(35):7190. |
| [6] | Butcher R J;Clark D L;Gordon J C et al.Synthesis and X-ray crystal structures of the samarium mono(pentamethylcyclopentadienyl) aryloxide complexes (η-C5Me5)Sm(O-26-t-Bu2C6H3)2(THF) and [(η-C5Me5)Sm(O-2,6-i-Pr2C6H3)3Li(THF)]. Differences in metathesis chemistry of 2,6-Di-iso-propylphenoxide and 2,6-di-tert-butylphenoxide ligands[J].Journal of Organometallic Chemistry,1999,577(02):228. |
| [7] | Taylor M D;Carter C P .Preparation of anhydrous lanthanide halides especially iodides[J].Journal of Radioanalytical and Nuclear Chemistry,1962,24(02):387. |
| [8] | Schaverien C J;Frijns J H G;Heeres H J.Monocyclopentadienyl yttrium Chemistry: incorporation of alkoxides as supporting ligands and synthesis of [Y(C5Me5)(OC6H3But2)(μ-H)]2[J].Journal of the Chemical Society,Chemical Communications,1991(06):642. |
| [9] | Hitchcock P B;Lappert M F;Smith R G .Tris(26-di-t-butylphenoxo) yttrium: a three-coordinate hydrocarbon-soluble aryloxide of yttrium[J].Inorganica Chimica Acta,1987,139(02):183. |
| [10] | Shannon R D .Revised effective ionic radii and systematic studies of interatomic distances in halides and chalcogenides[J].Acta Crystallographica Section A:Foundations of Crystallography,1976,32(02):751. |
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