Exploring the Versatility of N-Pyrazole, P-Phosphinite Hybrid Ligands against Pd(II). From Monomers and Dimers to One-Dimensional Chain, Two-Dimensional Layer Polymers and Three-Dimensio

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• 作者：Sergio Mu帽oz ; Miguel Guerrero ; Josep Ros ; Teodor Parella ; Merce Font-Bardia ; Josefina Pons
• 刊名：Crystal Growth & Design
• 出版年：2012
• 出版时间：December 5, 2012
• 年：2012
• 卷：12
• 期：12
• 页码：6234-6242
• 全文大小：603K
• 年卷期：v.12,no.12(December 5, 2012)
• ISSN：1528-7505

文摘

The versatility of N-pyrazole, P-phosphinite hybrid ligands [2-(3,5-dimethyl-1H-pyrazol-1-yl)ethyldiphenylphosphinite (L¹), 3-(3,5-dimethyl-1H-pyrazol-1-yl)propyldiphenylphosphinite (L²), and 2-(3,5-diphenyl-1H-pyrazol-1-yl)ethyldiphenylphosphinite (L³)] has been studied toward Pd(II). The reactions lead to a mixture of three complexes in solution for each ligand ([PdCl₂(L^x)], [PdCl₂(L^x)₂] and [PdCl₂(L^x)]₂) obtaining monomers (where L acts as mono-/bidentated agents) and dimers where the two L bridge the two metallic atoms in a head-to-tail arrangement. Complexes have been isolated and fully characterized by analytical and spectroscopic methods. X-ray crystal structures of some of the complexes as well as of other species [PdCl₂L³]₂ (only detected in the solid state) are presented. Furthermore, these complexes were prepared to examine the effects of the L structure on the topology and interpenetration form (one-dimensional chain, two-dimensional layer polymers and three-dimensional networks). Additionally, experimental and simulated NMR studies and a battery of modifications in the synthesis of the complexes (relation ratio of the starting products, order of addition, solvents and temperature) permit a better understanding of the role of ligands in the self-assembly process.