ORGANOMETALLIC COMPOUNDS OF THE LANTHANIDES .97. SYNTHESIS AND CRYSTAL STRUCTURES OF MONOMERIC BIS(ETHYLTETRAMETHYLCYCLOPENTADIENYL) AMIDE AND ALKYL DERIVATIVES OF THE LANTHANIDES

摘要

The trichlorides of yttrium, neodymium, samarium and lutetium react with 2 equiv. of Na[C(5)Me(4)Et] in THF to form [(C(5)Me(4)Et)(2)LnCl(THF)] (Ln = Y, 1; Nd, 2; Sm, 3; Lu, 4). Metathesis of 1-4 with NaN(SiMe(3))(2) and LiCH(SiMe(3))(2) in toluene gives [(C(5)Me(4)Et)(2)Ln{E(SiMe(3))(2)}] (E = N, Ln = Y, 5; Nd, 6; Sm, 7; Lu, 8; E = CH, Ln = Y, 9; Nd, 10; Sm, 11). The new compounds were characterized by elemental analysis and mass and NMR spectrometry. Additionally, X-ray structural analysis of 5 and 11 was performed. The silylamide 5 crystallized in the monoclinic space group C2/c with a = 9.169(2), b = 21.166(8), c = 15.625(3) Angstrom, beta = 94.15(2)degrees, V = 3025(2) Angstrom(3) and Z = 4. The final refinement resulted in R(1) = 2.86% (I > 4 sigma(I)). Compound 11 crystallized in the orthorhombic space group Pbca with a = 18.499(6), b = 14.181(6), c = 23.290(5) Angstrom, V = 6110(3) Angstrom(3), Z = 8, and R(1) = 3.04% (I > 4 sigma(I)). [References: 42]