Structure determination of a partially ordered layered silicate material with an NMR crystallography approach

2017 ◽  
Vol 73 (3) ◽  
pp. 184-190 ◽  
Author(s):  
Darren Henry Brouwer ◽  
Sylvian Cadars ◽  
Kathryn Hotke ◽  
Jared Van Huizen ◽  
Nicholas Van Huizen

Structure determination of layered materials can present challenges for conventional diffraction methods due to the fact that such materials often lack full three-dimensional periodicity since adjacent layers may not stack in an orderly and regular fashion. In such cases, NMR crystallography strategies involving a combination of solid-state NMR spectroscopy, powder X-ray diffraction, and computational chemistry methods can often reveal structural details that cannot be acquired from diffraction alone. We present here the structure determination of a surfactant-templated layered silicate material that lacks full three-dimensional crystallinity using such an NMR crystallography approach. Through a combination of powder X-ray diffraction and advanced 29Si solid-state NMR spectroscopy, it is revealed that the structure of the silicate layer of this layered silicate material templated with cetyltrimethylammonium surfactant cations is isostructural with the silicate layer of a previously reported material referred to as ilerite, octosilicate, or RUB-18. High-field 1H NMR spectroscopy reveals differences between the materials in terms of the ordering of silanol groups on the surfaces of the layers, as well as the contents of the inter-layer space.

2013 ◽  
Vol 117 (23) ◽  
pp. 12258-12265 ◽  
Author(s):  
Dmytro V. Dudenko ◽  
P. Andrew Williams ◽  
Colan E. Hughes ◽  
Oleg N. Antzutkin ◽  
Sitaram P. Velaga ◽  
...  

2010 ◽  
Vol 2010 ◽  
pp. 1-5 ◽  
Author(s):  
Neil A. Williams ◽  
Mahboub Merzouk ◽  
Peter B. Hitchcock

A range of silver iminoalkyl imidazol-2-ylidene complexes have been isolated in good yield (50%–85%) and characterised by and NMR spectroscopy. A single crystal X-ray diffraction structure determination of 1--(benzylhydrylidene-amino)-ethyl-benzyl imidazol-2-ylidene silver bromide indicated monodentate coordination of the ligand.


IUCrData ◽  
2017 ◽  
Vol 2 (12) ◽  
Author(s):  
Matthias Weil

The crystal structure of γ-TeO2was redetermined on the basis of single-crystal X-ray diffraction data. The previous structure determination of this modification was based on laboratory powder X-ray diffraction data [Champarnaud-Mesjardet al.(2000).J. Phys. Chem. Solids,61, 1499–1507]. The current redetermination revealed all atoms with anisotropic displacement parameters, accompanied with a much higher accuracy and precision in terms of bond lengths and angles, and the determination of the absolute structure. The crystal structure consists of TeO4bisphenoids that combine through corner-sharing of all their oxygen atoms into a three-dimensional framework.


2016 ◽  
Vol 16 (4) ◽  
pp. 1798-1804 ◽  
Author(s):  
Abigail E. Watts ◽  
Keisuke Maruyoshi ◽  
Colan E. Hughes ◽  
Steven P. Brown ◽  
Kenneth D. M. Harris

1994 ◽  
Vol 89 (7) ◽  
pp. 583-586 ◽  
Author(s):  
Toshihiro Shimada ◽  
Yukito Furukawa ◽  
Etsuo Arakawa ◽  
Kunikazu Takeshita ◽  
Tadashi Matsushita ◽  
...  

1985 ◽  
Vol 22 (2) ◽  
pp. 545-553 ◽  
Author(s):  
M. J. Musmar ◽  
Gary E. Martin ◽  
Robert T. Gampe ◽  
Vincent M. Lynch ◽  
Stanley H. Simonsen ◽  
...  

2016 ◽  
Vol 3 (11) ◽  
pp. 1351-1362 ◽  
Author(s):  
Zhengyang Zhou ◽  
Lukáš Palatinus ◽  
Junliang Sun

The combination of PXRD and ED is applied to determine modulated structures which resist solution by more conventional methods.


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