M[P(1,2-O 2C 6H 4) 3] (M = K or Na) - Synthesis, characterization, and use in halide abstraction

被引：0
作者：
Siu, Paul W. [1 ]
Gates, Derek P. [1 ]
机构：
[1] Department of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver
来源：
Canadian Journal of Chemistry | 2012年 / 90卷 / 07期
关键词：
Anions; Macrocycles; Palladium; Phosphorus; Rhodium;
D O I：
10.1139/v2012-028
中图分类号：
学科分类号：
摘要：
Alkali metal salts of the tris(o-phenylenedioxy)phosphate anion, K[P(1,2-O 2C 6H 4) 3] (K[1]) and Na[P(1,2-O 2C 6H 4) 3] (Na[1]), were prepared by treating Et 3NH[1] with KH or NaH, respectively. X-ray crystallographic analysis of K[1], crystallized in the presence of DMSO, revealed a dimeric structure of formulation K 2(DMSO) 6[1] 2·C 7H 8. In contrast, the crystal structure of K[1] grown from MeCN consists of fascinating hexagonal macrocycles with formulation {K(MeCN) 2[1]} 6 with an outside diameter of about 25 Å and a very small hole (≤2.5 Å). Remarkably, these hexagonal macrocycles stack one upon the other with a spacing of about 9.4 Å. The salt, K[1], is an effective halide abstraction agent reacting with (dppp)PdCl 2 (dppp = 1,3-bis(diphenylphosphino)propane) (1:1 ratio) or [(cod)RhCl] 2 (2:1 ratio) to afford [(dppp)Pd(μ-Cl)] 2 and (cod)Rh[1], respectively. The molecular structures of each complex were determined. © 2012 Published by NRC Research Press.
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页码：574 / 583
页数：9
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