CHEMISTRY OF ORGANOMETAL METALLACYCLIC SIDE-GROUP METAL-COMPOUNDS .8. SYNTHESIS AND PROPERTIES OF LI2PD(CH2(CH2)2CH2)2(D)X - MOLECULAR-STRUCTURE OF [LI(THF)2]2PD(CH2(CH2)2CH2)2

被引:15
作者
FROHLICH, HO [1 ]
WYRWA, R [1 ]
GORLS, H [1 ]
机构
[1] FRIEDRICH SCHILLER UNIV,MAX PLANCK GESELL,CO2 CHEM ARB,O-6900 JENA,GERMANY
关键词
D O I
10.1016/0022-328X(93)83308-I
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
[(Et2O)Li2Pd(CH2(CH2)2CH2)2] (1) was prepared by treatment of (1.5-COD)PdCl2 with Li(C4H8)Li in diethyl ether. By substituting other n-donor for the diethyl ether in 1, derivatives of the composition [(D)xLi2Pd(CH2(CH2)2CH2)2] (D=N.N, N',N'-tetrametbylethylenediamine (TMEDA), x = 2 (2); N,N,N',N',N''-pentamethyldiethylenetriamine (PMDETA), x = 2 (3); tetrahydrofuran (THF), x = 4 (4)) are obtained. The complexes 1-4 have been characterized by elemental and DTA analysis, and complexes 2 and 3 by H-1 and C-13 NMR spectroscopy as well. The crystal structure of 4 has been determined by an X-ray diffraction study. The crystal data and the final R values are as follows: space group P1BAR (Z = 1) with cell parameters a = 9.060(7) angstrom, b = 9.126(9) angstrom, c = 9.723(6) angstrom, alpha = 107.46(4)-degrees, beta = 91.20(4)-degrees, gamma = 116.23(3)-degrees, R = 0.041, R(w) = 0.050. The structural details are discussed. The first results of the reaction of 2 with CO are described, and IR investigation of the reaction mixture suggest that carbonyl cluster dianions of the composition [Pd3(CO)3(mu2-CO)3]n2- are present in solution. Other products of this reaction are 1-butylcyclopentanol, cyclopentanone and cyclopentanol.
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页码:7 / 12
页数:6
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