Macrocyclic amines as structure-directing agents for the synthesis of three-dimensional antimony-sulfide frameworks

被引:46
作者
Powell, AV [1 ]
Lees, RJE
Chippindale, AM
机构
[1] Heriot Watt Univ, Dept Chem, Edinburgh EH14 4AS, Midlothian, Scotland
[2] Univ Reading, Sch Chem, Reading RG6 6AD, Berks, England
基金
英国工程与自然科学研究理事会;
关键词
D O I
10.1021/ic060263f
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A new family of antimony sulfides, incorporating the macrocyclic tetramine 1,4,8,11-tetraazacyclotetradecane ( cyclam), has been prepared by a hydrothermal method. [C10N4H26][Sb4S7] (1), [Ni(C10N4H24)][Sb4S7] (2), and [Co(C10N4H24)](x)[C10N4H26](1-x)[Sb4S7] (0.08 <= x <= 0.74) (3) have been characterized by single-crystal X-ray diffraction, elemental analysis, thermogravimetry, and analytical electron microscopy. All three materials possess the same novel three-dimensional Sb4S72- framework, constructed from layers of parallel arrays of Sb4S84- chains stacked at 90 to one another. In 1, doubly protonated macrocyclic cations reside in the channel structure of the antimonysulfide framework. In 2 and 3, the cyclam acts as a ligand, chelating the divalent transition- metal cation. Analytical and X-ray diffraction data indicate that the level of metal incorporation in 2 is effectively complete, whereas in 3, both metalated and nonmetalated forms of the macrocycle coexist within the structure.
引用
收藏
页码:4261 / 4267
页数:7
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