Kim Sanghoon, Kim Jong Seung, Shon Ok Jae, Lee Shim Sung, Park Ki-Min, Kang Sang Ook, Ko Jaejung
Department of Chemistry, Korea University, Chochiwon, Chungnam 339-700, Korea.
Inorg Chem. 2004 May 3;43(9):2906-13. doi: 10.1021/ic030221g.
The preparation of an 1,3-alternate calix[4]arene phosphorus ligand, 25,27-bis(2-(diphenylphosphino)ethoxy)-26,28-bis(1-propyloxy)calix[4]arene (3), is presented. Ligand 3 is obtained in three steps in 64% overall yield. Reaction of 3 with [Rh(cot)2]BF4 produced the encapsulated rhodium complex [Rh[(P,P)-diphen-calix[4]arene]]BF4 (4). As revealed by a single-crystal X-ray diffraction study, the rhodium center has a bent coordination environment with a P-Rh-P angle of 135.66(3) degrees. Palladation of 3 employing Pd(MeCN)42 yielded the chelate palladium complex 7 in which the palladium center has a slightly bent configuration. Treatment of the ligand with Pd(cod)Cl2 and [Pd(eta3-C4H7)(THF)2]BF4 leads to the isolation of the monometallic complex. Full characterization includes X-ray structural studies of compounds 3, 4, and 6.
本文介绍了一种1,3-交替杯[4]芳烃磷配体，即25,27-双(2-(二苯基膦基)乙氧基)-26,28-双(1-丙氧基)杯[4]芳烃(3)的制备方法。配体3通过三步反应得到，总产率为64%。3与[Rh(cot)2]BF4反应生成包封铑配合物[Rh[(P,P)-二苯-杯[4]芳烃]]BF4(4)。单晶X射线衍射研究表明，铑中心具有弯曲的配位环境，P-Rh-P角为135.66(3)度。用Pd(MeCN)42对3进行钯化反应，得到螯合钯配合物7，其中钯中心具有轻微弯曲的构型。用Pd(cod)Cl2和[Pd(η3-C4H7)(THF)2]BF4处理该配体，得到单金属配合物。完整的表征包括对化合物3、4和6的X射线结构研究。
