SYNTHESIS OF YTTRIUM AND LANTHANIDE SILYLOXY COMPLEXES FROM ANHYDROUS NITRATE AND OXO ALKOXIDE PRECURSORS AND THE X-RAY CRYSTAL-STRUCTURE OF [CE(OSIPH3)3(THF)3](THF)

被引：64

作者：

GRADEFF, PS ^{[1
]}

YUNLU, K ^{[1
]}

DEMING, TJ ^{[1
]}

OLOFSON, JM ^{[1
]}

DOEDENS, RJ ^{[1
]}

EVANS, WJ ^{[1
]}

机构：

[1] UNIV CALIF IRVINE,DEPT CHEM,IRVINE,CA 92717

来源：

INORGANIC CHEMISTRY | 1990年 / 29卷 / 03期

关键词：

D O I：

10.1021/ic00328a016

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The anhydrous trivalent nitrates (NH4)xLn(NO3)3+x(Ln = Y, Ce, Nd, Pr), prepared by heating Ln(NO3)3(H2O)), in the presence of NH4NO3, react with 3 + x equiv of NaOSiPh3in THF to form [Ln(OSiPh3)3(THF)3](THF) complexes. The cerium complex crystallizes from THF at −30 °C in the monoclinic space group P21with unit cell dimensions a = 14.679 (2) Å, b = 16.432 (3) Å, c = 15.021 (3) Å, β = 115.86 (1.2)°, and Z = 2. Least-squares refinement of the model based on 6685 reflections (F2> 3.0Ã(F2)) converged to a final RF= 0.033. The six oxygen-bound ligands describe a fac-octahedral geometry around cerium with average Ce-O(OSiPh3) and Ce-O(THF) distances of 2.222 (4) and 2.591 (4) Å, respectively. Crystals of the Ln = Pr and Y complexes have very similar unit cell dimensions. The anhydrous tetravalent nitrate (NH4)2Ce(NO3)6reacts with 6 equiv of (a) NaOSiPh, in DME to form Ce(OSiPh3)4(DME) and (b) NaOSiEt3in CH3CN to form Ce(OSiEt3)4. (NH4)3Y(NO3)6reacts with NaOiPr in 2-propanol to form Y5(OiPr)O, which reacts with Ph3SiOH to form [Y(OSiPh3)3(THF)3](THF). © 1990, American Chemical Society. All rights reserved.

引用

页码：420 / 424

页数：5

共 43 条

[1] SYNTHESIS AND CRYSTAL-STRUCTURE OF A NEODYMIUM ISOPROPOXIDE CHLORIDE, ND6[OCH(CH3)2]17CL [J].