Transition-Metal Complexes Containing Parent Phosphine or Phosphinyl Ligands and Their Use as Precursors for Phosphide Nanoparticles
作者:Susanne Bauer、Cornelia Hunger、Michael Bodensteiner、Wilfried-Solo Ojo、Arnaud Cros-Gagneux、Bruno Chaudret、Céline Nayral、Fabien Delpech、Manfred Scheer
DOI:10.1021/ic5012082
日期:2014.11.3
transition-metal complexes were synthesized without using hazardous PH3 gas in good yields by photolysis of the transition-metal carbonyl complexes M(CO)6-x (M = Cr, W, Fe; x = 0, 1) in tetrahydrofuran followed by reaction with P2(SiMe3)4 and subsequent methanolysis to give the bridging complexes [(CO)xM(μ-PH2)]2 (M = Fe, x = 3 (1), M = Cr, x = 4 (2a), M = W, x = 4 (2b)). The photolysis of [(CO)4M(μ-PH2)]2 (M =
通过光解过渡金属羰基配合物M(CO)6- x(M = Cr,W,Fe; x = 0,1),可以不使用有害的PH 3气体以高收率合成具有P–H功能的过渡金属配合物在四氢呋喃中反应以P 2(森达3)4和随后的甲醇分解,得到桥接配合物[(CO)X M(μ-PH 2)] 2(M =铁,X = 3(1),M =铬,x = 4(2a),M = W,x = 4(2b))。[(CO)4的光解M(μ-PH 2)] 2(M 2 = CR(图2a),M = W(图2b))与P(森达3)3涂布,随后甲醇合成PH 2桥接过渡金属双核与终端PH络合物3组。产物[(CO)4 M(μ-PH 2)2 M(CO)3(PH 3)](M =铬(图3a),M = W(图3B))和[(CO)4 W(μ- PH 2)2 W(CO)2(PH 3)2 ](4b)以中等产量分离。这类化合物的另一种合成方法是络合物[(CO)3 M(PH 3)3