Highly stable and porous porphyrin-based zirconium and hafnium phosphonates - electron crystallography as an important tool for structure elucidation

Chemical Science
Timo RhauderwiekNorbert Stock

Abstract

The Ni-metallated porphyrin-based tetraphosphonic acid (Ni-tetra(4-phosphonophenyl)porphyrin, Ni-H8TPPP) was used for the synthesis of highly porous metal phosphonates containing the tetravalent cations Zr4+ and Hf4+. The compounds were thoroughly characterized regarding their sorption properties towards N2 and H2O as well as thermal and chemical stability. During the synthesis optimization the reaction time could be substantially decreased under stirring from 24 to 3 h in glass vials. M-CAU-30, [M2(Ni-H2TPPP)(OH/F)2]·H2O (M = Zr, Hf) shows exceptionally high specific surface areas for metal phosphonates of aBET = 1070 and 1030 m2 g-1 for Zr- and Hf-CAU-30, respectively, which are very close/correspond to the theoretical values of 1180 and 1030 m2 g-1. CAU-30 is always obtained as mixtures with one mol ZrO2/HfO2 per formula unit as proven by TEM, electron diffraction, TG and elemental analysis. Hence experimentally derived specific surface areas are 970 and 910 m2 g-1, respectively. M-CAU-30 is chemically stable in the pH range 0 to 12 in HCl/NaOH and thermally up to 420 °C in air as determined by variable-temperature powder X-ray diffraction (VT-PXRD). The crystal structure of M-CAU-30 was determined by combining electron diff...Continue Reading

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Citations

Feb 9, 2019·Chemical Communications : Chem Comm·Yunus ZorluGündoğ Yücesan
May 16, 2019·Angewandte Chemie·Sebastian LeubnerNorbert Stock
Jun 4, 2019·Chemistry : a European Journal·Maria MaaresGündoğ Yücesan
May 17, 2019·Chemistry : a European Journal·Yulia Y EnakievaAslan Y Tsivadze
Feb 14, 2020·Dalton Transactions : an International Journal of Inorganic Chemistry·Stephan WöhlbrandtNorbert Stock
Feb 14, 2020·Dalton Transactions : an International Journal of Inorganic Chemistry·S LeubnerN Stock
Apr 16, 2020·Chemistry : a European Journal·Yunus ZorluGündoğ Yücesan
Aug 25, 2020·Acta Crystallographica Section B, Structural Science, Crystal Engineering and Materials·Ute KolbSergi Plana-Ruiz
Sep 23, 2020·Chemical Communications : Chem Comm·Song-Song BaoLi-Min Zheng
Jun 25, 2020·Nature Communications·Patrik TholenGündoğ Yücesan
Jan 12, 2021·Dalton Transactions : an International Journal of Inorganic Chemistry·Siddhartha DeAlexandra Fateeva
Feb 23, 2021·Chemical Society Reviews·Zhigang HuDan Zhao
Apr 6, 2019·Journal of the American Chemical Society·Dahae SongNak Cheon Jeong
Nov 16, 2021·Dalton Transactions : an International Journal of Inorganic Chemistry·Ge-Hua WenLi-Min Zheng

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Methods Mentioned

BETA
electron diffraction
transmission electron microscopy
X-ray

Software Mentioned

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Powdercell
Materials
SIR2014
Python
DIAMOND
Materials Studio
TOPAS Academic
ADT3D
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