Gajecki Leah, Twamley Brendan, Berg David J
Department of Chemistry, University of Victoria, PO Box 1700 Stn CSC, Victoria, BC V8W 2Y2, Canada.
School of Chemistry, Trinity College Dublin, University of Dublin, Dublin 2, Ireland.
Acta Crystallogr E Crystallogr Commun. 2020 Apr 21;76(Pt 5):703-709. doi: 10.1107/S2056989020005034. eCollection 2020 May 1.
Reaction of 2-(4,4-dimethyl-2-oxazolin-2-yl)aniline (H-) with one equivalent of Na[N(SiMe)] in toluene afforded pale-yellow crystals of tetra-meric poly[bis-[μ-2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido][μ-2-(4,4-dimethyl-2-oxa-zolin-2-yl)aniline]tetra-sodium(I)], [Na(CHNO)] or [Na(H-)] (), in excellent yield. Subsequent reaction of [Na(H-)] () with 1.33 equivalents of anhydrous YbCl 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(CHNO)] or Yb(H-) () in moderate yield. Direct reaction of three equivalents of 2-(4',4'-dimethyl-2'-oxazolin-yl)aniline (H-) with Yb[N(SiMe)] in toluene resulted in elimination of hexa-methyl-disilazane, HN(SiMe), and produced Yb(H-) () in excellent yield. The structure of consists of tetra-meric Na(H-) subunits in which each Na cation is bound to two H- 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 consists of a distorted octa-hedron where the bite angle of ligand 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 to an oxazoline nitro-gen while for the other two oxazoline N atoms are to each other. This results in a significantly longer Yb-N(oxazoline) distance [2.468 (3) Å] for the bond to the anilide compared to those for the oxazoline N atoms to one another [2.376 (3), 2.390 (3) Å].
2-(4,4-二甲基-2-恶唑啉-2-基)苯胺(H-)与一当量的Na[N(SiMe)]在甲苯中反应，以优异的产率得到四聚体聚双-[μ-2-(4,4-二甲基-2-恶唑啉-2-基)苯胺基][μ-2-(4,4-二甲基-2-恶唑啉-2-基)苯胺]四钠(I)，[Na(CHNO)]或Na(H-)的淡黄色晶体。Na(H-)与1.33当量的无水YbCl在甲苯-四氢呋喃50:50的混合物中随后反应，以中等产率得到三-[2-(4,4-二甲基-2-恶唑啉-2-基)苯胺基]镱(III)，[Yb(CHNO)]或Yb(H-)的黄色晶体。三当量的2-(4',4'-二甲基-2'-恶唑啉基)苯胺(H-)与Yb[N(SiMe)]在甲苯中直接反应导致六甲基二硅氮烷HN(SiMe)消除，并以优异的产率生成Yb(H-)]()。的结构由四聚体Na(H-)亚基组成，其中每个Na阳离子与两个H-桥连双齿配体结合，并且这些亚基通过四个恶唑啉O原子中的两个桥连到相邻四聚体中的Na阳离子而连接成聚合物链。这导致每个四聚体单元内有两个4配位和两个5配位的Na阳离子。的结构由一个扭曲的八面体组成，其中配体的咬角在74.72 (11)和77.79 (11)度之间。恶唑啉(和酰苯胺)N原子占据子午位置，使得对于一个配体，一个酰苯胺氮与一个恶唑啉氮相对，而对于另外两个恶唑啉N原子彼此相对。这导致与彼此相对的恶唑啉N原子的键[2.376 (3)，2.390 (3) Å]相比，与酰苯胺的键的Yb-N(恶唑啉)距离[2.468 (3) Å]明显更长。
