Journal of Fluorine Chemistry ( IF 1.9 ) Pub Date : 2020-01-30 , DOI: 10.1016/j.jfluchem.2020.109475 E.I. Voit , N.A. Didenko , A.V. Gerasimenko , A.B. Slobodyuk
The synthesis and study of the structure and properties (by methods of X-ray structural analysis, DTA, IR, Raman, and 1H, 19F NMR, including 19F MAS NMR) of a new crystal hydrate of the composition ZnZr2F10∙6H2O (1) have been performed.
The compound 1 crystallizes in the monoclinic system with the following unit cell parameters: a = 6.5628(2), b = 10.2031(4), c = 9.0965(4) Å, β = 100.532(1)°, sp.gr. C2/m, Z = 2. The crystal structure is built of flat cross-linked anion layers of the composition and octahedral [Zn(H2O)6]2+ cations. The complex cations and anions are linked in the structure into a three-dimensional network by O–H···F and O–H···O hydrogen bonds.
It has been established that decomposition of 1 in temperature range 50-850 °C in air proceeds stepwise through the following stages: ZnZr2F10∙6H2O → ZnZr2F10∙4H2O → ZnZr2F10∙2H2O → ZnZr2OF8 with formation of the mixture of the final products ZnO and ZrO2. The vibrational and NMR spectroscopy data for the initial compound and intermediate products of its decomposition have been obtained, systematized, and summarized.
中文翻译:
晶体ZnZr 2 F 10 ∙6H 2 O的合成与络合物研究
组成为ZnZr 2 F的新型晶体水合物的合成和结构和性能研究(通过X射线结构分析,DTA,IR,拉曼和1 H,19 F NMR,包括19 F MAS NMR)已执行10 ∙6H 2 O(1)。
化合物1在单斜晶系统中具有以下晶胞参数结晶:a = 6.5628(2),b = 10.2031(4),c = 9.0965(4)Å,β = 100.532(1)°,sp.gr. C2 / m,Z =2。晶体结构由组成平坦的交联阴离子层组成和八面体[Zn(H 2 O)6 ] 2+阳离子。复杂的阳离子和阴离子在结构中通过OH···F和OH···O氢键连接成三维网络。
已经确定,在空气中温度范围为50-850°C的1中,分解过程逐步进行:ZnZr 2 F 10 ∙6H 2 O→ZnZr 2 F 10 ∙4H 2 O→ZnZr 2 F 10 ∙2H 2 O→ZnZr 2 OF 8形成最终产物ZnO和ZrO 2的混合物。已获取,系统化和总结了其分解的初始化合物和中间产物的振动和NMR光谱数据。