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Oxidation in Nonclassical Organolanthanide Chemistry: Synthesis, Characterization, and X-ray Crystal Structures of Cerium(III) and -(IV) Amides
[Ce(NR2)3] (R = SiMe3) with TeCl 4 in tetrahydrofuran solution gave a mixture of two major products in a combined yield of ca. 50% based on available metal: (i) the Ce(IV) amide [CeCl(NR2)3] (1), which was isolated as purple needles and identified on the basis of 1H NMR and mass spectra, microanalysis, and a single-crystal X-ray analysis [C18H 54CeClN3Si6, rhombohedral, R3c (No. 161), a = b = 18.4508(7) A, c = 16.8934(7) A, Z = 6]; (ii) unstable [{Ce(NR2)2(mu-Cl)(thf)}2] (2), as colorless blocks [C32H88Ce2Cl2N 4O2Si8, monoclinic, P21/n (No. 14), a = 14.506(3) A, b = 13.065(3) A, c = 16.779(3) A, beta = 113.789(12) A, Z = 2], which readily disproportionated in solution. In toluene solution, the product 1 was obtained exclusively. The same cerium(III) amide starting material was oxidized by PBr2Ph 3 in diethyl ether solution to give purple [CeBr(NR2) 3] (3) [C18H54BrCeN3Si6, rhombohedral, R3c (No. 161), a = b = 18.4113(12) A, c = 16.9631(17) A, Z = 6], along with presumed [CeBr3(OEt2) n], which has not been characterized but with thf, by displacement of the ether ligands, gave [CeBr3(thf)4] (4) [C 16H32Br3CeO4, triclinic, P1 (No. 2), a = 8.2536(7) A, b = 9.4157(5) A, c = 15.5935(14) A, alpha = 79.009(5), beta = 87.290(3), gamma = 74.835(5), Z = 2). TeBr4 reacted with [Ce(NR2)3] in thf to give small amounts of 3; the major product (although only formed in 15% yield) was monomeric [CeBr2(NR2)(thf)3] (5) [C 18H42Br2CeNO3Si2, monoclinic, P21/c (No. 14), a = 14.9421(4) A, b = 11.8134(5) A, c = 15.8317(7) A, alpha = gamma = 120, beta = 92.185(3), Z = 4].
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Phosphine ligand,
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate