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We appreciate support from the group of Prof Dr. Sonnichsen (University of Kiel) for NMR measurements and thank Dr. Helge Reinsch (CAU Kiel) and Dr. Michael Wharmby (DESY) for helpful discussions. The financial support by the province of Schleswig-Holstein is highly appreciated.

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Synthesis, Structure, and Characterization of Defect-free [Hf6(μ3-O)4(μ3-OH)4(C4H2O4)6] (Hf-UiO-66-Fum)

Publicat a:Zeitschrift Fur Anorganische Und Allgemeine Chemie. 644 (24): 1771-1776 - 2018-12-31 644(24), DOI: 10.1002/zaac.201800338

Autors: Jacobsen, Jannick; Gosch, Jonas; Stock, Norbert

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The reaction of HfCl4 with fumaric acid (C4H4O4, H(2)Fum) in a DMF/HCOOH solvent mixture at 120 degrees C for 24 h results in the formation of a defect-free sample of Hf-UiO-66-Fum with UiO-66 structure type. Treatment of the (as)-synthesized sample in boiling ethanol followed by a thermal treatment at 70 degrees C leads to a sample of composition [Hf-6(mu(3)-O)(4)(mu(3)-OH)(4)(Fum)(6)]center dot 18H(2)O center dot 2EtOH. In the crystal structure the hexanuclear clusters {Hf-6(mu(3)-O)(4)(mu(3)-OH)(4)} are twelve-fold connected by C4H2O42- ions to form the framework with the fcu topology. This cluster connectivity was confirmed by a combination of characterization techniques methods, i.e. CHN analyses, N-2 sorption as well as H-1-NMR spectroscopic and thermogravimetric measurements. The MOF shows a thermal stability of T = 390 degrees C, a specific BET surface area of 389 m(2)center dot g(-1) and a water uptake of 204 mg center dot g(-1). The crystal structure was determined from powder X-ray diffraction (PXRD) data, employing the Rietveld method. The compound crystallizes in the cubic space group Pn3 and is isostructural to Zr-UiO-66-Fum. Only a small increase of the lattice parameter a from 17.8309(4) to 17.87978(14) angstrom is observed.

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