Search results for "Solid-State"

Charged Bis-Cyclometalated Iridium(III) Complexes with Carbene-Based Ancillary Ligands

2013

Charged cydometalated (CN) iridium(III) complexes with carbene-based ancillary ligands are a promising family of deep-blue phosphorescent compounds. Their emission properties are controlled primarily by the main CN ligands, in contrast to the classical design of charged complexes where NN ancillary ligands with low-energy pi* orbitals, such as 2,2'-bipyridine, are generally used for this purpose. Herein we report two series of charged iridium complexes with various carbene-based ancillary ligands. In the first series the CAN ligand is 2-phenylpyridine, whereas in the second one it is 2-(2,4-difluorophenyl)-pyridine. One biscarbene (:CC:) and four different pyridine carbene (NC:) chelators a…

Square wave voltammetric determination of the redox state of a reversibly oxidized/reduced depolarizer in solution and in solid state

2012

Abstract Square wave voltammetric measurements allows for determining the composition of system containing a reversibly reducible/oxidable electroactive species in two oxidation states. The method is based on recording the ratio of reverse to forward peak currents. That ratio can be correlated with the molar fraction of the oxidized (or reduced) form of the depolarizer. The method was compared with cyclic voltammetric methods suggested in literature and it was tested using Fe ( CN ) 6 3 - / Fe ( CN ) 6 4 - in solution phase. Application to solid state systems is illustrated by the dehydroindigo/indigo couple in synthetic Maya Blue-type specimens prepared from indigo plus different clays whe…

Resonance ionization mass spectrometry for ultratrace analysis of plutonium with a new solid state laser system

2004

Abstract Resonance ionization mass spectrometry (RIMS) is well-suited for isotope selective ultratrace analysis of long-lived radioactive isotopes due to its high element and isotope selectivity and good sensitivity. For the analysis of plutonium with a pulsed RIMS apparatus, a powerful, reliable and easy to handle Nd:YAG pumped titanium–sapphire laser system has been developed and combined with a time-of-flight mass spectrometer. Spectroscopic measurements led to an efficient three step excitation and ionization scheme for plutonium with λ1 = 420.76 nm, λ2 = 847.28 nm, and λ3 = 767.53 nm. The isotope shifts in this scheme for the plutonium isotopes 238 Pu through 244 Pu have been determine…

X-ray structures of five variably tert-butoxycarbonyl-substituted adenines and their liquid and solid state NMR investigations

2009

Abstract Adenine reacts selectively with di- tert -butyldicarbonate in THF in the presence of NaOH to give N 9-monoBoc-adenine 1 . The molecular structure and crystal packing of this and four other variably substituted Boc-derivatives of adenine were determined in solid state by means of X-ray diffraction and CP/MAS NMR experiments and characterized in liquid state by 1 H, 13 C, and 15 N NMR spectroscopy as well. Additionally, crystal structure of inclusion compound between N 6 -monoBoc-adenine 5 and CHCl 3 is reported. Tautomeric equilibria of mono- and disubstituted derivatives 4 and 5 in liquid state were studied by VT NMR experiments.

Nuclear Magnetic Resonance and Electron Spin Resonance Spectroscopy

2001

The article contains sections titled: 1. Introduction 2. Principles of Magnetic Resonance 2.1. Nuclear and Electronic Properties 2.2. Nuclei and Electrons in a Stationary Magnetic Field 2.3. Basic Principles of the NMR and ESR Experiments 2.4. Relaxation 3. High-Resolution Solution NMR Spectroscopy 3.1. The NMR Experiment 3.1.1. Continuous Wave Methodology 3.1.2. Fourier Transform Methodology 3.2. Spectral Parameters 3.2.1. Chemical Shift 3.2.2. Spin - Spin Coupling 3.2.3. Signal Intensity 3.2.4. Relaxation Times 3.3. NMR and Structure 3.3.1. Hydrogen (1H and 2H) 3.3.2. Carbon (13C) 3.3.3. Fluorine (19F) 3.3.4. Phosphorus (31P) 3.3.5. Nitrogen (14N and 15N) 3.3.6. Oxygen (17O) 3.3.7. Silico…

ChemInform Abstract: “Supramolecular” Solid-State Chemistry: Interpenetrating Diamond-Type Frameworks of U4+ Ions Linked by S,S′-Bidentate P2S2-6 Mol…

2010

Performance of a thermoelectric module based on n-type (La0.12Sr0.88)0.95TiO3-δ and p-type Ca3Co4-xO9+δ

2020

Here, we present the performance of a thermoelectric (TE) module consisting of n-type (La0.12Sr0.88)0.95TiO3 and p-type Ca3Co4-xO9+δ materials. The main challenge in this investigation was operation of TE module in different atmosphere conditions, since n-type has its optimum TE-performance at reducing, while p-type at oxidizing conditions. The TE module was exposed to two different atmospheres and demonstrated higher stability in N2 atmosphere than in air. The maximum electrical power output decreased after 40 h when the hot side was exposed to N2 at 600 °C, while only 1 h at 400 °C in ambient air was enough to oxidize (La0.12Sr0.88)0.95TiO3 followed by a reduced electrical power output. T…

Order-disorder evolution in solid solutions of the NLO material KTiOPO : K Rb TiOPO and K Rb TiOPO in the temperature range 293-973 K

2000

K0.88Rb0.12TiOPO4 and K0.465Rb0.535TiOPO4 solid solutions of the potassium titanyl phosphate (KTiOPO4, space group Pna21) family, are described at 293, 473, 673, 873 and at 973 K. Their high resolution structures are obtained by using accurate single-crystal X-ray diffraction techniques at high resolution, (sin A-1. Large anharmonic motion of alkaline ions increasing with temperature allows the evolution of the rubidium and potassium ions repartition in the two alkaline sites versus temperature. To describe this motion inducing ionic conductivity phenomenon and to determine accurately the order-disorder evolution, two alkaline site refinement models are developed and discussed. A thermodyna…

Structural investigation of four-centre photopolymerisation of bis-phthalamic bis-chalcone derivative in the crystalline state

1997

By combining the results obtained from an electron diffraction tilting series with solid state NMR and powder X-ray diffraction, it was possible to determine the unit cell parameters and space group of BPABC crystals grown from DMAA solution both before and after irradiation. Subsequently semi-empirical quantum mechanical and packing energy calculations led to a model structure which agreed well with all the electron diffraction data and thus provided insight into the cross-linking mechanism. © 1997 John Wiley & Sons Ltd.

Isomerism in [MCl2(ERR‘)2] (M = Pd, Pt; E = S, Se; R, R‘ = Me, Ph)

2006

A series of thioether and selenoether complexes [MCl2(EPh2)2] and [MCl2(SMePh)2] (M = Pt, Pd; E = S, Se) have been prepared and characterized to explore the isomerism of the complexes in solution and in the solid state. The NMR spectroscopic information indicates that only one isomer is present in solution in case of the palladium complexes, while two isomers are formed in the case of most platinum complexes. Single-crystal X-ray structures of trans-[PdCl2(SPh2)2] (1t), trans-[PdCl2(SePh2)2] (2t), cis-[PtCl2(SePh2)2] (4c), trans-[PdCl2(SMePh)2] (5t), and trans-[PtCl2(SMePh)2] (7t) are reported and have been used as starting points for the X-ray powder diffraction structure determinations us…