A novel Zn(4)O-based triazolyl benzoate MOF: synthesis, crystal structure, adsorption properties and solid state 13C NMR investigations.

A novel Zn(4)O-based triazolyl benzoate MOF: synthesis, crystal structure, adsorption properties and solid state 13C NMR investigations.
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DOI:
10.1039/c1dt11431j
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发表时间:
2012-01
影响因子:
4
通讯作者:
Jörg Lincke;Daniel Lässig;Karolin Stein;Jens Moellmer;Anusree Viswanath Kuttatheyil;C. Reichenbach;A. Moeller;R. Staudt;G. Kalies;M. Bertmer;H. Krautscheid
Jörg Lincke;Daniel Lässig;Karolin Stein;Jens Moellmer;Anusree Viswanath Kuttatheyil;C. Reichenbach;A. Moeller;R. Staudt;G. Kalies;M. Bertmer;H. Krautscheid
中科院分区:
化学2区
文献类型:
--
作者:
Jörg Lincke;Daniel Lässig;Karolin Stein;Jens Moellmer;Anusree Viswanath Kuttatheyil;C. Reichenbach;A. Moeller;R. Staudt;G. Kalies;M. Bertmer;H. Krautscheid

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新合成的Zn(4)O基MOF(3)(∞)[Zn(4)(μ(4)-O){(Metrz-pba)(2)mPh}(3)]·8DMF(1·8DMF)具有43%的孔隙率和高达430 °C的显着热稳定性。单晶X射线结构分析可以使用合成的晶体以及去溶剂化的晶体进行。除了单晶的溶剂热合成外,还报道了MOF微晶材料的可规模化合成。结合TG-MS和固态NMR测量揭示了移动的DMF分子在骨架的孔系统中的存在。吸附测量证实,在77 K的孔隙结构是完全可访问的氮分子。吸附孔体积为0.41 cm(3)g(-1),与单晶结构估算的孔体积0.43 cm(3)g(-1)具有很好的相关性。
The newly synthesized Zn(4)O-based MOF (3)(∞)[Zn(4)(μ(4)-O){(Metrz-pba)(2)mPh}(3)]·8 DMF (1·8 DMF) of rare tungsten carbide (acs) topology exhibits a porosity of 43% and remarkably high thermal stability up to 430 °C. Single crystal X-ray structure analyses could be performed using as-synthesized as well as desolvated crystals. Besides the solvothermal synthesis of single crystals a scalable synthesis of microcrystalline material of the MOF is reported. Combined TG-MS and solid state NMR measurements reveal the presence of mobile DMF molecules in the pore system of the framework. Adsorption measurements confirm that the pore structure is fully accessible for nitrogen molecules at 77 K. The adsorptive pore volume of 0.41 cm(3) g(-1) correlates well with the pore volume of 0.43 cm(3) g(-1) estimated from the single crystal structure.