双苯甲酰羟胺-钨酰螯合物的分子结构与晶体结构

THE MOLECULAR STRUCTURE AND CRYSTAL STRUCTURE OF TUNGSTYL-BISBENZOHYDROXAMATE CHELATE COMPOUND

苯甲酰羟胺(CHCONHOH)对钨钼配位效率高,速度快,生成的配合物稳定.在一定的酸性条件下,对钨钼萃取具有较好的分离性能.等及Agrawal曾报道该类钨钼配合物均易被高级醇定量萃取,可用于分光光度法测定微量钨和钼.但对配位过程的研究,特别是对配合物结构与性能的研究则未见报道.本文在钨配合物组成、红外光谱、多晶X光衍射等研究的基础上培养其单晶,并测定了晶体结构,试图对其性能研究提供一些信息.实验与结构分析配合物(CHON)WO由钨酸钠与苯甲酰羟胺混合的水溶液,在pH-1~6时,用己醇

The crystal structure of(CHON)WOwas determined on a Syntex-R3 four-circle diffractometer with X-ray intensity data collected inθ~2θscanning mode.The space group is C~2-P6,withα=17.38(2),c=10.872(8)■,Z=6.The position of tungsten atom was revealed by Patterson function and direct method.Then the parameters of the remaining non-H atoms were found from Fourier and difference Fourier syntheses.Refinement was carried out by block-diagonal matrix least-squares procedure.The structure was refined to a final R value of 0.0558.The investigation confirms that W(Ⅵ)is coordinated in a distorted octahedron by six oxygen.The chelate rings surrounding W(Ⅵ)are planar five-member rings.The lengths of C—C bonds connecting chelate rings and their respective benzene rings are shorter than normal C—C bond.The angles between these two planar rings are not large.It is possible that a part ofπelectrons in these two conjugated system are able to overlap each other.