Solid-state EPR strategies for the structural characterization of paramagnetic NO adducts of frustrated Lewis pairs (FLPs)

2015 ◽  
Vol 142 (12) ◽  
pp. 124201 ◽  
Author(s):  
Marcos de Oliveira ◽  
Thomas Wiegand ◽  
Lisa-Maria Elmer ◽  
Muhammad Sajid ◽  
Gerald Kehr ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Frustrated Lewis Pairs ◽  
Lewis Pairs

scholarly journals Solid-State NMR Techniques for the Structural Characterization of Cyclic Aggregates Based on Borane–Phosphane Frustrated Lewis Pairs

Molecules ◽  
2020 ◽  
Vol 25 (6) ◽  
pp. 1400 ◽  
Author(s):  
Robert Knitsch ◽  
Melanie Brinkkötter ◽  
Thomas Wiegand ◽  
Gerald Kehr ◽  
Gerhard Erker ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Solid State Nmr ◽  
Magic Angle ◽  
Frustrated Lewis Pairs ◽  
Wide Range ◽  
Nmr Techniques ◽  
Nmr Methods ◽  
Lewis Pairs

Modern solid-state NMR techniques offer a wide range of opportunities for the structural characterization of frustrated Lewis pairs (FLPs), their aggregates, and the products of cooperative addition reactions at their two Lewis centers. This information is extremely valuable for materials that elude structural characterization by X-ray diffraction because of their nanocrystalline or amorphous character, (pseudo-)polymorphism, or other types of disordering phenomena inherent in the solid state. Aside from simple chemical shift measurements using single-pulse or cross-polarization/magic-angle spinning NMR detection techniques, the availability of advanced multidimensional and double-resonance NMR methods greatly deepened the informational content of these experiments. In particular, methods quantifying the magnetic dipole–dipole interaction strengths and indirect spin–spin interactions prove useful for the measurement of intermolecular association, connectivity, assessment of FLP–ligand distributions, and the stereochemistry of adducts. The present review illustrates several important solid-state NMR methods with some insightful applications to open questions in FLP chemistry, with a particular focus on supramolecular associates.

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

1999 ◽  
Vol 121 (10) ◽  
pp. 2307-2308 ◽  
Author(s):  
T. Beringhelli ◽  
G. D'Alfonso ◽  
M. Panigati ◽  
F. Porta ◽  
P. Mercandelli ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Methyl Group ◽  
Metal Atoms

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

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
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.

Manganese(i) poly(mercaptoimidazolyl)borate complexes: spectroscopic and structural characterization of Mn⋯H–B interactions in solution and in the solid state

2005 ◽  
pp. 171-180 ◽  
Author(s):  
Leigh A. Graham ◽  
Alison R. Fout ◽  
Karl R. Kuehne ◽  
Jennifer L. White ◽  
Bhaskar Mookherji ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Borate Complexes
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