Search results for "Spectroscopy"
showing 10 items of 10293 documents
Reversible Dimerization of Tetraureas Derived from Calix[4]Arenes
1999
Calix[4]arene derivatives, substituted at the wider rim by four urea functions are easily available in great variety. In apolar solvents like benzene or chloroform they dimerize via NH…O=C hydrogen bonds encapsulating a single solvent molecule as guest. The exclusive formation of dimers has been proved in solution by NMR, while their shape has been characterized by single crystal X-ray analysis. The kinetic stability and the rate of the guest exchange have been studied by NOESY experiments using a derivative with lower symmetry.
Valence-Delocalized and Valence-Trapped FeIIFeIII Complexes: Drastic Influence of the Ligands
1997
The two macrocyclic ligands H 2 L 1 and H 2 L 2 are not very different, but their Fe II Fe III complexes are remarkably so. [L 1 Fe 2 (μ-OAc) 2 ](ClO 4 ) is valence-delocalized on the Mossbauer time scale over the range 1.8-364 K, whereas [L 2 Fe 2 (μ-OAc)(OAc)(H 2 O)](ClO 4 )·2H 2 O is valence-trapped even at room temperature. The difference in properties of these complexes is also reflected in their electronic spectra, in their electrochemical and magnetic behavior, and in their structures.
Spin crossover in iron(II) tris(2-(2′-pyridyl)benzimidazole) complex monitored by variable temperature methods: synchrotron powder diffraction, DSC, …
2003
Abstract The thermal expansion of the spin crossover system [Fe(pybzim) 3 ](ClO 4 ) 2 · H 2 O (pybzim=2-(2 ′ -pyridyl)benzimidazole) has been determined from powder X-ray data between 50 and 250 K; the wavelength of the synchrotron source was 1.21888(1) A. The unit cell parameters of the triclinic crystal system were a =12.091 A, b =12.225 A, c =14.083 A, α =77.70°, β =80.35°, γ =74.35°, and V =1944.9 A 3 at 250 K. In addition to the linear thermal expansion of the unit cell volume, an extra expansion due to the low-spin (LS) to high-spin (HS) transition is observed. The V ( T ) function shows a sudden increase comparable with the step in the effective magnetic moment at the transition reg…
Stoichiometry of LiNiO2 Studied by Mössbauer Spectroscopy
2002
From the 61Ni and 57Fe Mossbauer spectroscopy data follows the cationic site assignment in Li1−x Ni1+x O2. Our data explain the ferromagnetic properties of this material because of the appearance of Ni2+ (S = 1) among Ni3+ (S = 1/2) in Ni3+O2 hexagonal planes. We have no evidence for the ferromagnetic interaction between the NiO2 layers through the excess Ni2+ ions substituting the Li+ ions. The presence of Ni2+ found in the Ni3+O2 planes explains the absence of the Jahn-Teller distortions probably because of the electronic transfer between the Ni3+ and Ni2+ ions.
Unravelling the fine structure of stacked bipyridine diamine-derived C-3-discotics as determined by X-ray diffraction, quantum-chemical calculations,…
2011
An in depth investigation of the fine structure adopted by the helical stacks of C3-discotics 1 incorporating three 3,3'-diamino-2,2'-bipyridine units is described. In the bulk the molecules display liquid crystalline behaviour in a temperature window of >300 K and an ordered rectangular columnar mesophase (Colro) with an inter-disc distance of 3.4 Å is assigned. X-Ray diffraction on aligned samples has also revealed a helical superstructure in the liquid crystalline state, and a rotation angle of 13–16° between consecutive discs. The proposed superstructure in the bulk phase has been further substantiated by a combination of quantum-chemical calculations and solid-state NMR spectroscopy…
Detailed study of defects in thin fullerite films
2012
The structural investigations of fullerite films were performed using high-resolution electron microscopy, electron diffraction and electron energy loss spectroscopy and X-ray photoelectron spectroscopy. In particular defects such as dislocations, stacking faults and twins were studied in details. It was shown that fullerite films could be characterized by a face-centered cubic (f.c.c.) structure with lattice parameter a = 1.416 nm. They are distinguished for their rich polytypic structure that is caused by breaking of alteration of closely packed planes of (111) type. The quantitative method based on information theory using the “run-length encoding” algorithm was suggested to evaluate the…
Competitive gold-activation modes in terminal alkynes: an experimental and mechanistic study.
2013
The competition between π- and dual σ,π-gold-activation modes is revealed in the gold(I)-catalyzed heterocyclization of 1-(o-ethynylaryl)urea. A noticeable effect of various ligands in gold complexes on the choice of these activation modes is described. The cationic [Au(IPr)](+) (IPr=2,6-bis(diisopropylphenyl)imidazol-2-ylidene) complex cleanly promotes the π activation of terminal alkynes, whereas [Au(PtBu3 )](+) favors intermediate σ,π species. In this experimental and mechanistic study, which includes kinetic and cross-over experiments, several σ-gold, σ,π-gold, and other gold polynuclear reaction intermediates have been isolated and identified by NMR spectroscopy, X-ray diffraction, or …
Solid state NMR studies of gels derived from low molecular mass gelators
2016
The emergence of NMR crystallography provides a unique opportunity to study solids, gels and xerogels, thereby providing ample information to elucidate molecular packing in the native gel. This review details the importance as well as the application of solid state NMR spectroscopy combined with other analytical tools to study gels derived from low molecular mass organo- and hydrogelators.
Alternating Chain Magnetism in Catena-μ-Oxo-Hemiporphyrazinatoiron(IV), The First μ-Oxo Linear Chain Complex Of Iron
1984
Abstract X-ray studies, Mossbauer, and magnetism show FeOHp to be an antiferromagneticaly coupled alternating chain with J = -133 cm−1, g = 2.3 and an alternation parameter of 0.4.
EXAFS study of the local structure of crystalline and nanocrystalline Y2O3using evolutionary algorithm method
2015
Temperature-dependent local structure and lattice dynamics of yttria (Y2O3) were studied by X-ray absorption spectroscopy. Novel method, which combines the reverse Monte Carlo and evolutionary algorithm techniques, was applied for the analysis of extended X-ray absorption fine structure at the Y K-edge. This approach allowed us to reconstruct 3D atomic structure models of crystalline and nanocrystalline Y2O3.