Department of Chemistry, King Saud University, P. O. Box 2455, Riyadh 11451, Saudi Arabia.
Molecules. 2010 May 17;15(5):3618-33. doi: 10.3390/molecules15053618.
An investigation into the potential ruthenium(II) 1-3 complexes of type [RuCl(2)(P)(2)(N)(2)] using triphenylphosphine and 1,3-bis-diphenylphosphinepropane and 3-(triethoxysilyl)propylamine has been carried out at room temperature in dichloromethane under an inert atmosphere. The structural behaviors of the phosphine ligands in the desired complexes during synthesis were monitored by (31)P{(1)H}-NMR. The structure of complexes 1-3 described herein has been deduced from elemental analyses, infrared, FAB-MS and (1)H-, (13)C- and (31)P-NMR spectroscopy. Xerogels X1-X3 were synthesized by simple sol-gel process of complexes 1-3 using tetraethoxysilane as co-condensation agent in methanol/THF/water solution. Due to their lack of solubility, the structures of X1-X3 were determined by solid state (13)C-, (29)Si- and (31)P-NMR spectroscopy, infrared spectroscopy and EXAFS.
已经在室温下,在惰性气氛中,于二氯甲烷中,对钌(II)1-3 型配合物[RuCl2(P)2(N)2]的潜在的钌(II)1-3 配合物进行了研究,使用三苯基膦和 1,3-双二苯基膦丙烷以及 3-(三乙氧基硅基)丙胺。在合成过程中,通过(31)P{(1)H}-NMR 监测所需配合物中膦配体的结构行为。本文所描述的配合物 1-3 的结构是通过元素分析、红外、FAB-MS 和(1)H、(13)C 和(31)P-NMR 光谱学推断出来的。通过使用四乙氧基硅烷作为共缩合剂,在甲醇/THF/水溶液中,通过简单的溶胶-凝胶法合成了 Xerogels X1-X3。由于它们缺乏溶解性,因此通过固态(13)C-、(29)Si-和(31)P-NMR 光谱学、红外光谱学和 EXAFS 来确定 X1-X3 的结构。