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Published March 9, 2021 | Supplemental Material
Journal Article Open

Further Investigations of Racemic and Chiral Molecular Sieves of the STW Topology

Abstract

Large single crystals of pure-silica STW-type molecular sieves are prepared using 1,2,3,4,5-pentamethylimidazolium (12345PMI) and 2-ethyl-1,3,4-trimethylimidazolium (2E134TMI) as organic structure-directing agents (OSDAs) and α-amino acid additives. The effects of the amount and type of amino acid on the crystallization of pure-silica STW materials are investigated. Room-temperature single-crystal X-ray diffractometry shows that 12345PMI better fits the STW cage than 2E134TMI and is fully consistent with computed simulations. The synthesis of an enantioenriched R-STW-type molecular sieve having a Si/Ge ratio of 2.2 is achieved using a chiral, dicationic OSDA that contains two stereocenters. The conformation of the chiral OSDA in the chiral framework has been obtained from a Rietveld refinement using synchrotron powder diffraction data and is the first structure refinement of an enantioenriched, inorganic molecular sieve prepared from a pure, asymmetric OSDA.

Additional Information

© 2021 American Chemical Society. Received: November 28, 2020; Revised: February 9, 2021; Published: February 24, 2021. The Chevron Energy and Technology Company offered financial support for this research. J.H.K. and M.E.D. thank Prof. George R. Rossman (Geochemistry, Caltech) and Lawrence M. Henling (Beckman Institute, Caltech) for the polarized optical microscopy and the single-crystal X-ray diffractometry analyses, respectively. M.W.D. thanks the U.S. Department of Energy (DOE) for financial support under contract DE-SC0019324. J.H.K. thanks Dr. Marcella Lusardi for acquiring the FT-IR spectrum of the R-STW germanosilicate sample. L.B.M and C.B. thank Nicola Casati for the synchrotron powder diffraction measurements on the Materials Science beamline at the SLS in Villigen, Switzerland. Author Contributions: The manuscript was written through the contributions of all authors. All authors have given approval to the final manuscript. The authors declare no competing financial interest.

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Supplemental Material - cm0c04573_si_001.pdf

Supplemental Material - cm0c04573_si_002.cif

Supplemental Material - cm0c04573_si_003.cif

Supplemental Material - cm0c04573_si_004.cif

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Created:
August 20, 2023
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