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使用导数差最小化的粉末衍射晶体结构分析:1-(四唑-5-基)-2-硝基胍钾盐的实例

Powder diffraction crystal structure analysis using derivative difference minimization: example of the potassium salt of 1-(tetrazol-5-yl)-2-nitroguanidine.

作者信息

Solovyov Leonid A, Astachov A M, Molokeev M S, Vasiliev A D

机构信息

Institute of Chemistry and Chemical Technology, 660049 Krasnoyarsk, Russia.

出版信息

Acta Crystallogr B. 2005 Aug;61(Pt 4):435-42. doi: 10.1107/S0108768105015004. Epub 2005 Jul 19.

Abstract

The crystal structure of the potassium salt of 1-(tetrazol-5-yl)-2-nitroguanidine [K(C2H3N8O2)] was solved and refined from X-ray powder diffraction data by applying the derivative difference minimization (DDM) method. The compound is of interest as an energetic substance. The structure model was found from a Patterson search. The reflection intensities for the Patterson synthesis were derived from the powder profile by applying a newly developed DDM-based profile decomposition procedure. The use of the DDM method allowed successful location and unconstrained refinement of all the atomic positions, including those of three independent H atoms. The advantages of DDM in terms of the precision and reproducibility of the structural parameters are discussed in comparison to Rietveld refinement results. The failure to refine the H-atom positions by the Rietveld method was attributed to systematic errors associated with the background modelling, which are avoided by DDM.

摘要

通过应用导数差最小化(DDM)方法,从X射线粉末衍射数据中解析并精修了1-(四唑-5-基)-2-硝基胍钾盐[K(C₂H₃N₈O₂)]的晶体结构。该化合物作为一种含能材料备受关注。通过帕特森搜索找到结构模型。通过应用新开发的基于DDM的轮廓分解程序,从粉末轮廓中得出帕特森合成的反射强度。DDM方法的使用使得所有原子位置,包括三个独立氢原子的位置都能成功定位并进行无约束精修。与里特韦尔德精修结果相比,讨论了DDM在结构参数精度和可重复性方面的优势。里特韦尔德方法未能精修氢原子位置归因于与背景建模相关的系统误差,而DDM避免了这些误差。

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