[锗（7）氧（13）氢氧根（2）氟（3）](3)(-)·氯（-）·2[镍（二乙三胺）（2）](2+)：首例由过渡金属配合物模板化的链状锗酸盐

[Ge(7)O(13)(OH)(2)F(3)](3)(-).Cl(-).2[Ni(dien)(2)](2+): the first chainlike germanate templated by a transition metal complex.

作者信息

Zhang Hong-Xia, Zhang Jie, Zheng Shou-Tian, Yang Guo-Yu

机构信息

Coordination and Hydrothermal Chemistry Group, State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, China.

出版信息

Inorg Chem. 2003 Oct 20;42(21):6595-7. doi: 10.1021/ic034645m.

DOI:10.1021/ic034645m

PMID:14552607

Abstract

The first chainlike germanate, Ge(7)O(13)(OH)(2)F(3)(-).Cl(-).2Ni(dien)(2), has been solvothermally synthesized by using Ni(dien)(2)(2+) cations as the template and characterized by IR, SEM, TGA, powder X-ray diffraction (PXRD), energy-dispersive X-ray analysis (EDXA), elemental analysis, and single-crystal X-ray diffraction, respectively. This compound crystallized in the monoclinic space group P2/nwith a = 8.8904(2) A, b = 17.4374(3) A, c = 13.2110(3) A, beta = 101.352(1) degrees, V = 2007.97(7) A(3), and Z = 2. Interestingly, the structure contains two types of chiral mer-Ni(dien)(2) cations and two types of chiral chains, one left-handed and the other right-handed, which lead to a racemic compound. The orderly separation of achiral s-fac-Ni(dien)(2) and chiral mer-Ni(dien)(2) isomers was found in the structure. The structure is stabilized by N-H.O(F, Cl) hydrogen bonds.

摘要

首个链状锗酸盐Ge(7)O(13)(OH)(2)F(3)(-)·Cl(-)·2Ni(dien)(2)已通过以Ni(dien)(2)(2+)阳离子为模板进行溶剂热合成，并分别通过红外光谱(IR)、扫描电子显微镜(SEM)、热重分析(TGA)、粉末X射线衍射(PXRD)、能量色散X射线分析(EDXA)、元素分析和单晶X射线衍射进行了表征。该化合物结晶于单斜空间群P2/n中，a = 8.8904(2) Å，b = 17.4374(3) Å，c = 13.2110(3) Å，β = 101.352(1)°，V = 2007.97(7) Å(3)，Z = 2。有趣的是，该结构包含两种手性顺式-Ni(dien)(2)阳离子和两种手性链，一种左旋，另一种右旋，这导致了一种外消旋化合物。在该结构中发现了非手性面式-Ni(dien)(2)和顺式-Ni(dien)(2)异构体的有序分离。该结构通过N-H…O(F, Cl)氢键得以稳定。