Abstract
Reaction of 2-(4,4-dimethyl-2-oxazolin-2-yl)aniline (H2-L1) with one equivalent of Na[N(SiMe3)2] in toluene afforded pale-yellow crystals of tetra-meric poly[bis-[μ3-2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido][μ2-2-(4,4-dimethyl-2-oxa-zolin-2-yl)aniline]tetra-sodium(I)], [Na4(C11H13N2O)4] n or [Na4(H-L1)4] n (2), in excellent yield. Subsequent reaction of [Na4(H-L1)4] n (2) with 1.33 equivalents of anhydrous YbCl3 in a 50:50 mixture of toluene-THF afforded yellow crystals of tris-[2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido]ytterbium(III), [Yb(C11H13N2O)3] or Yb(H-L1)3 (3) in moderate yield. Direct reaction of three equivalents of 2-(4',4'-dimethyl-2'-oxazolin-yl)aniline (H2-L1) with Yb[N(SiMe3)2]3 in toluene resulted in elimination of hexa-methyl-disilazane, HN(SiMe3)2, and produced Yb(H-L1)3 (3) in excellent yield. The structure of 2 consists of tetra-meric Na4(H-L1)4 subunits in which each Na+ cation is bound to two H-L1 bridging bidentate ligands and these subunits are connected into a polymeric chain by two of the four oxazoline O atoms bridging to Na+ cations in the adjacent tetra-mer. This results in two 4-coordinate and two 5-coordinate Na+ cations within each tetra-meric unit. The structure of 3 consists of a distorted octa-hedron where the bite angle of ligand L1 ranges between 74.72 (11) and 77.79 (11) degrees. The oxazoline (and anilide) N atoms occupy meridional sites such that for one ligand an anilide nitro-gen is trans to an oxazoline nitro-gen while for the other two oxazoline N atoms are trans to each other. This results in a significantly longer Yb-N(oxazoline) distance [2.468 (3) Å] for the bond trans to the anilide compared to those for the oxazoline N atoms trans to one another [2.376 (3), 2.390 (3) Å].