CHEMISTRY OF ORGANOMETAL METALLACYCLIC SI DE-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
Ho. Frohlich et al., CHEMISTRY OF ORGANOMETAL METALLACYCLIC SI DE-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, Journal of organometallic chemistry, 456(1), 1993, pp. 7-12
[(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 h
ave 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 da
ta and the final R values are as follows: space group P1BAR (Z = 1) wi
th 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 det
ails 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- ar
e present in solution. Other products of this reaction are 1-butylcycl
opentanol, cyclopentanone and cyclopentanol.