Multinuclear NMR and Powder X-ray Diffraction Studies of Si and Sn Clathrates of Alkali Metals: Vacancies, Disorder and Knight Shifts

2001 ◽  
Vol 691 ◽  
Author(s):  
Michael J. Ferguson ◽  
Igor L. Moudrakovski ◽  
Christopher I. Ratcliffe ◽  
John S. Tse
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Alkali Metals ◽  
Rietveld Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Binary Metal ◽  
Knight Shifts

ABSTRACTThe Structure I type binary metal clathrates of K/Si, Rb/Si and Cs/Sn have been synthesised and studied by powder X-ray diffraction and solid state NMR. Rietveld analysis shows that in all three materials some of the cages are empty, and that in the Cs/Sn clathrate there are vacancies in the Sn framework. The NMR results yield Knight shifts for 29Si and 39K and confirm that the Cs/Sn clathrate is not conducting. Many of the features of the NMR spectra can be understood in terms of the distributions of atom vacancies.

scholarly journals The Silicides YT2Si2 (T =Co, Ni, Cu, Ru, Rh, Pd): A Systematic Study by 89Y Solid-state NMR Spectroscopy

2014 ◽  
Vol 69 (3) ◽  
pp. 305-312 ◽  
Author(s):  
Christoph Höting ◽  
Hellmut Eckert ◽  
Samir F. Matar ◽  
Ute Ch. Rodewald ◽  
Rainer Pöttgen
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Arc Melting ◽  
Bonding Interaction ◽  
Fermi Edge ◽  
Extra Electron ◽  
Knight Shifts ◽  
Structure Calculations

The ThCr2Si2-type silicides YT2Si2 (T =Co, Ni, Cu, Ru, Rh, Pd) were synthesized from the elements by arc-melting. They were characterized by powder X-ray diffraction, and the structures were refined on the basis of single-crystal X-ray diffractometer data. The course of the lattice parameters shows a distinct anomaly for YRu2Si2 which has by far the smallest c/a ratio along with elongated Y- Si distances. Systematic 89Y solid-state NMR spectra show large Knight shifts arising from unpaired conduction electron spin density near the Fermi edge. The Knight shift decreases with increasing valence electron count (VEC), reflecting the sensitivity of this parameter to electronic properties. The particularly strong structural distortion observed in YRu2Si2 manifests itself in a sizeable magnetic shielding anisotropy. Electronic structure calculations for YRu2Si2 and YRh2Si2 reveal similar projected density of states (PDOS) shapes with an energy upshift of the Fermi level in YRh2Si2 due to the extra electron brought in by Rh. As a consequence, the PDOS at the Fermi energy is twice as large in the Ru compound as in the Rh compound. While both compounds show the major bonding interaction within the T2Si2 layers, YRh2Si2 exhibits significantly stronger Y-Si bonding

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

Gallium-containing Heusler phases ScRh2Ga, ScPd2Ga, TmRh2Ga and LuRh2Ga – magnetic and solid state NMR-spectroscopic characterization

2017 ◽  
Vol 72 (8) ◽  
pp. 609-615
Author(s):  
Lukas Heletta ◽  
Stefan Seidel ◽  
Christopher Benndorf ◽  
Hellmut Eckert ◽  
Rainer Pöttgen
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Spectroscopic Characterization ◽  
Structural Disorder ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
Phase Purity ◽  
X Ray ◽  
Arc Melting ◽  
Pauli Paramagnetism

AbstractThe gallium-containing Heusler phases ScRh2Ga, ScPd2Ga, TmRh2Ga and LuRh2Ga have been synthesized by arc-melting of the elements followed by different annealing sequences to improve phase purity. The samples have been studied by powder X-ray diffraction. The structures of Lu0.97Rh2Ga1.03 (Fm3̅m, a=632.94(5) pm, wR2=0.0590, 46 F2 values, seven variables) and Sc0.88Rh2Ga1.12 (a=618.91(4) pm, wR2=0.0284, 44 F2 values, six variables) have been refined from single crystal X-ray diffractometer data. Both gallides show structural disorder through Lu/Ga and Sc/Ga mixing. Temperature dependent magnetic susceptibility measurements showed Pauli paramagnetism for ScRh2Ga, ScPd2Ga, and LuRh2Ga and Curie-Weiss paramagnetism for TmRh2Ga. 45Sc and 71Ga solid state MAS NMR spectroscopic investigations of the Sc containing compounds confirmed the site mixing effects typically observed for Heusler phases. The data indicate that the effect of mixed Sc/Ga occupancy is significantly stronger in ScRh2Ga than in ScPd2Ga.

The Adsorption and Chemistry of Tripropyl phosphate (TPP) into Microporous and Mesoporous NaX Zeolites

2011 ◽  
Vol 1304 ◽  
Author(s):  
Qingguo Meng ◽  
David C. Doetschman ◽  
Apostolos K. Rizos ◽  
Min-Hong Lee ◽  
Jürgen T. Schulte ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Properties ◽  
Nmr Spectra ◽  
Nitrogen Adsorption ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nax Zeolite ◽  
Stoichiometric Amount ◽  
Polydiallyldimethylammonium Chloride ◽  
Adsorption Analysis

ABSTRACTAdsorption and chemistry of tripropylphosphate (TPP) in mesoporous NaX zeolite, which was templated by cationic templated polymer (polydiallyldimethylammonium chloride, PDADMAC) with two different length chains, was investigated. The structural properties of the zeolites were characterized by X-ray diffraction (XRD) and nitrogen adsorption analysis. The chemical activities of different zeolites toward the decomposition of TPP were determined with solid state 31P NMR spectra. After exposure of zeolites to TPP was sufficient and equilibrium was reached, a stoichiometric amount of water was also adsorbed and hydrolysis was observed. The TPP decomposition yields in different NaX zeolites were compared.

Packing Interactions in Hydrated and Anhydrous Forms of the Antibiotic Ciprofloxacin: a Solid-State NMR, X-ray Diffraction, and Computer Simulation Study

2011 ◽  
Vol 134 (1) ◽  
pp. 71-74 ◽  
Author(s):  
Luís Mafra ◽  
Sérgio M. Santos ◽  
Renée Siegel ◽  
Inês Alves ◽  
Filipe A. Almeida Paz ◽  
...  
Keyword(s):  
Computer Simulation ◽  
Solid State ◽  
Simulation Study ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
Computer Simulation Study ◽  
X Ray ◽  
Packing Interactions

Solid-state NMR and powder X-ray diffraction studies on ammonium ion-exchanged and dealuminated zeolite YNU-5

2020 ◽  
Vol 302 ◽  
pp. 110197
Author(s):  
Takuji Ikeda ◽  
Yuka Yoshida ◽  
Naoto Nakazawa ◽  
Satoshi Inagaki ◽  
Yoshihiro Kubota
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Ammonium Ion ◽  
X Ray Diffraction ◽  
X Ray
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