A structure refinement strategy for NMR crystallography: An improved crystal structure of silica-ZSM-12 zeolite from 29Si chemical shift tensors

Brouwer, Darren H.

doi:10.1016/j.jmr.2008.06.020

Cited by 65 publications

(23 citation statements)

References 70 publications

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“…It seems that many former (and in some cases well established) crystallographic data need to be revised in light of the new information brought about by ''NMR crystallography'' methods. 128,135,136 Strategies for structure determination based on first-principles methods have been proposed as a means of complementing/correcting previous diffraction results or to address new structures not accessible to conventional diffraction experiments (see Ref. 137 and references therein).…”

Section: Mg Nmrmentioning

confidence: 99%

Recent Advances in Solid-State 25Mg NMR Spectroscopy

Freitas

Smith

2012

Annual Reports on NMR Spectroscopy

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Section: Mg Nmrmentioning

confidence: 99%

Recent Advances in Solid-State 25Mg NMR Spectroscopy

Freitas

Smith

2012

Annual Reports on NMR Spectroscopy

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“…These integrated structure determination strategies in which solid-state NMR spectroscopy plays a crucial, but not exclusive, role is broadly referred to as NMR crystallography. [1] One class of materials for which NMR crystallography strategies have had success are zeolites [2][3][4][5][6][7] and layered network materials. [8][9][10][11] We originally demonstrated [2] that pure silica zeolite framework structures can be solved from 29 Si double quantum (DQ) dipolar recoupling NMR experiments given the following input information: (i) crystallographic space group, (ii) unit cell parameters, (iii) number and occupancies of Si sites, (iv) Si-O-Si connectivities between sites, and (v) longer range distance information found in the set of intersite 29 Si DQ build-up curves.…”

Section: Introductionmentioning

confidence: 99%

NMR crystallography of zeolites: How far can we go without diffraction data?

Brouwer

Huizen

2018

Magnetic Reson in Chemistry

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Nuclear magnetic resonance (NMR) crystallography-an approach to structure determination that seeks to integrate solid-state NMR spectroscopy, diffraction, and computation methods-has emerged as an effective strategy to determine structures of difficult-to-characterize materials, including zeolites and related network materials. This paper explores how far it is possible to go in determining the structure of a zeolite framework from a minimal amount of input information derived only from solid-state NMR spectroscopy. It is shown that the framework structure of the fluoride-containing and tetramethylammonium-templated octadecasil clathrasil material can be solved from the 1D Si NMR spectrum and a single 2D Si NMR correlation spectrum alone, without the space group and unit cell parameters normally obtained from diffraction data. The resulting NMR-solved structure is in excellent agreement with the structures determined previously by diffraction methods. It is anticipated that NMR crystallography strategies like this will be useful for structure determination of other materials, which cannot be solved from diffraction methods alone.

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“…211, 213, 236, 336, 337, 338, 339, 340, 341, 342 and for inorganic solids. 343,344 The ability of NMR chemical shifts to provide high quality structural information is demonstrated in these instances where other approaches or methods are equally useful and agreement among the results provides corroboration. With the increased confidence in shielding interpretation, it is timely to show that NMR shielding tensors can indeed provide unique structural information.…”

Section: Shielding Tensors As Tools For Nmr Crystallographymentioning

confidence: 91%

“…343 and ITQ-4,347 zeolites have been obtained by optimizing Si-O, O-O and Si-Si distances to reach a closer agreement between calculated and experimental 29 Si chemical shift tensors. The 17 O and 29 Si shielding in MgSiO 3 and Mg 2 SiO 4 have been studied by Ashbrook et al, allowing for a full assignment of the 17 O sites and a deeper understanding of how the 17 O shielding depends on the Si-O bond length and coordination environment.…”

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confidence: 98%