Modern solid state double resonance NMR strategies for the structural characterization of adsorbate complexes involved in the MTG process

Solid-state NMR spectroscopy is an established experimental technique which is used for the characterization of structural and dynamic properties of materials in their native state. Many types of solid-state NMR experiments have been used to characterize both lithium-based and sodium-based solid polymer and polymer–ceramic hybrid electrolyte materials. This review describes several solid-state NMR experiments that are commonly employed in the analysis of these systems: pulse field gradient NMR, electrophoretic NMR, variable temperature T1 relaxation, T2 relaxation and linewidth analysis, exchange spectroscopy, cross polarization, Rotational Echo Double Resonance, and isotope enrichment. In this review, each technique is introduced with a short description of the pulse sequence, and examples of experiments that have been performed in real solid-state polymer and/or hybrid electrolyte systems are provided. The results and conclusions of these experiments are discussed to inform readers of the strengths and weaknesses of each technique when applied to polymer and hybrid electrolyte systems. It is anticipated that this review may be used to aid in the selection of solid-state NMR experiments for the analysis of these systems.

Download Full-text

ChemInform Abstract: CRYSTALLIZATION AND SOLID-STATE STRUCTURAL CHARACTERIZATION OF (2,2′-BIPYRIDYL)ZINC TETRACARBONYLIRON, (BPY)ZNFE(CO)4

Chemischer Informationsdienst ◽

10.1002/chin.198045070 ◽

1980 ◽

Vol 11 (45) ◽

Author(s):

R. J. NEUSTADT ◽

T. H. CYMBALUK ◽

R. D. ERNST ◽

F. W. JUN. CAGLE

Keyword(s):

Solid State ◽

Structural Characterization

Download Full-text

A Methyl Group Bridging on Three Metal Atoms. Solid-State and Solution Structural Characterization of the [Re3(μ-H)3(μ3-CH3)(CO)9]-Anion

Journal of the American Chemical Society ◽

10.1021/ja983379m ◽

1999 ◽

Vol 121 (10) ◽

pp. 2307-2308 ◽

Cited By ~ 5

Author(s):

T. Beringhelli ◽

G. D'Alfonso ◽

M. Panigati ◽

F. Porta ◽

P. Mercandelli ◽

...

Keyword(s):

Solid State ◽

Structural Characterization ◽

Methyl Group ◽

Metal Atoms

Download Full-text

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

Journal of Porphyrins and Phthalocyanines ◽

10.1142/s1088424611004440 ◽

2012 ◽

Vol 16 (01) ◽

pp. 154-162 ◽

Cited By ~ 24

Author(s):

Edwin W.Y. Wong ◽

Daniel B. Leznoff

Keyword(s):

Absorption Spectrum ◽

Solid State ◽

Single Crystal ◽

Structural Characterization ◽

Heterometallic Complex ◽

State Structure ◽

Solid State Structure ◽

X Ray ◽

X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Download Full-text