Rietveld Refinement of MIL‐160 and Its Structural Flexibility Upon H2O and N2 Adsorption

The porous metal‐organic framework (MOF) MIL‐160 [Al(OH)(O2C‐C4H2O‐CO2)] was investigated by means of high‐resolution powder X‐ray diffraction experiments using synchrotron radiation. The structures of the dehydrated, hydrated and nitrogen loaded forms of MIL‐160 are refined by the Rietveld method....

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Vydáno v:European journal of inorganic chemistry Ročník 2018; číslo 32; s. 3626 - 3632
Hlavní autoři: Wahiduzzaman, Mohammad, Lenzen, Dirk, Maurin, Guillaume, Stock, Norbert, Wharmby, Michael T.
Médium: Journal Article
Jazyk:angličtina
Vydáno: Weinheim Wiley Subscription Services, Inc 31.08.2018
Témata:
Adsorption
Aluminium MOFs
Aluminum
Dehydration
Density functional calculations
Diffraction
Flexibility
Heat treatment
Inorganic chemistry
Lattice parameters
Mathematical analysis
Metal-organic frameworks
NMR
Nuclear magnetic resonance
Phase transitions
Rietveld method
Synchrotron powder diffraction
Synchrotron radiation
Water chemistry
Water sorption
X-ray diffraction
ISSN:1434-1948, 1099-0682
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Abstract The porous metal‐organic framework (MOF) MIL‐160 [Al(OH)(O2C‐C4H2O‐CO2)] was investigated by means of high‐resolution powder X‐ray diffraction experiments using synchrotron radiation. The structures of the dehydrated, hydrated and nitrogen loaded forms of MIL‐160 are refined by the Rietveld method. The structure of the hydrated form, as postulated from solid state NMR and DFT calculations, is confirmed. The host–guest and thermal responses of this compound are also investigated. Adsorption of water is found to induce a phase transition from I41/amd (the dehydrated structure) to I41md (the hydrated structure), mediated by flexibility of the MOF framework. Water molecules were observed to arrange themselves with an ice‐like geometry. Conversely, adsorption of more weakly interacting N2 into the structure or thermal treatment (cooling the sample from 400 to 80 K) leads to no phase transition, indicating that the phase transition is induced by the strong interactions of H2O with the framework. The accuracy of the refined structures is investigated by DFT calculations, which show very small deviations in optimised atomic positions and lattice parameters. The structure of Al‐MOF MIL‐160 [Al{OH(O2C‐C4H2O‐CO2)}], postulated from solid state NMR and DFT calculations, is confirmed by Rietveld refinement of high‐resolution synchrotron powder X‐ray diffraction. Its H2O and N2 host–guest complexes were also refined & demonstrate structural flexibility. DFT calculations demonstrate the high‐accuracy of the refined structures.
AbstractList The porous metal‐organic framework (MOF) MIL‐160 [Al(OH)(O2C‐C4H2O‐CO2)] was investigated by means of high‐resolution powder X‐ray diffraction experiments using synchrotron radiation. The structures of the dehydrated, hydrated and nitrogen loaded forms of MIL‐160 are refined by the Rietveld method. The structure of the hydrated form, as postulated from solid state NMR and DFT calculations, is confirmed. The host–guest and thermal responses of this compound are also investigated. Adsorption of water is found to induce a phase transition from I41/amd (the dehydrated structure) to I41md (the hydrated structure), mediated by flexibility of the MOF framework. Water molecules were observed to arrange themselves with an ice‐like geometry. Conversely, adsorption of more weakly interacting N2 into the structure or thermal treatment (cooling the sample from 400 to 80 K) leads to no phase transition, indicating that the phase transition is induced by the strong interactions of H2O with the framework. The accuracy of the refined structures is investigated by DFT calculations, which show very small deviations in optimised atomic positions and lattice parameters. The structure of Al‐MOF MIL‐160 [Al{OH(O2C‐C4H2O‐CO2)}], postulated from solid state NMR and DFT calculations, is confirmed by Rietveld refinement of high‐resolution synchrotron powder X‐ray diffraction. Its H2O and N2 host–guest complexes were also refined & demonstrate structural flexibility. DFT calculations demonstrate the high‐accuracy of the refined structures.
The porous metal‐organic framework (MOF) MIL‐160 [Al(OH)(O2C‐C4H2O‐CO2)] was investigated by means of high‐resolution powder X‐ray diffraction experiments using synchrotron radiation. The structures of the dehydrated, hydrated and nitrogen loaded forms of MIL‐160 are refined by the Rietveld method. The structure of the hydrated form, as postulated from solid state NMR and DFT calculations, is confirmed. The host–guest and thermal responses of this compound are also investigated. Adsorption of water is found to induce a phase transition from I41/amd (the dehydrated structure) to I41md (the hydrated structure), mediated by flexibility of the MOF framework. Water molecules were observed to arrange themselves with an ice‐like geometry. Conversely, adsorption of more weakly interacting N2 into the structure or thermal treatment (cooling the sample from 400 to 80 K) leads to no phase transition, indicating that the phase transition is induced by the strong interactions of H2O with the framework. The accuracy of the refined structures is investigated by DFT calculations, which show very small deviations in optimised atomic positions and lattice parameters.
Author Wharmby, Michael T.
Maurin, Guillaume
Stock, Norbert
Wahiduzzaman, Mohammad
Lenzen, Dirk
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SubjectTerms Adsorption
Aluminium MOFs
Aluminum
Dehydration
Density functional calculations
Diffraction
Flexibility
Heat treatment
Inorganic chemistry
Lattice parameters
Mathematical analysis
Metal-organic frameworks
NMR
Nuclear magnetic resonance
Phase transitions
Rietveld method
Synchrotron powder diffraction
Synchrotron radiation
Water chemistry
Water sorption
X-ray diffraction
Title Rietveld Refinement of MIL‐160 and Its Structural Flexibility Upon H2O and N2 Adsorption
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