Experimental NMR and MS study of benzoylguanidines. Investigation of E/Z isomerism

Molecules containing the guanidinic nuclei possess several pharmacological applications, and knowing the preferred isomers of a potential drug is important to understand the way it operates pharmacologically. Benzoylguanidines were synthesized in satisfactory to good yields and characterized by NMR, Electrospray Ionization Mass Spectrometry (ESI‐MS) and Fourrier Transform InfraRed Spectroscopy techniques (FTIR). E/Z isomerism of the guanidines was studied and confirmed by NMR analysis in solution (¹H‐¹³C Heteronuclear Single Quantum Coherence (HSQC) and Heteronuclear Multiple‐Bond Correlation (HMBC), ¹H‐¹⁵N HMBC, ¹H‐¹H Correlation Spectroscopy (COSY) and Nuclear Overhauser Effect Spectroscopy (NOESY) experiments) at low temperatures. Compounds with p‐Cl and p‐Br aniline moiety exist mainly as Z isomer with a small proportion of E isomer, whereas compounds with p‐NO2 moiety showed a decrease in proportion of isomer Z. The results are important for the application of these molecules as enzymatic inhibitors. Copyright © 2013 John Wiley & Sons, Ltd.     

Tellurium delta‐doped InGaP layers grown by metalorganic vapour phase epitaxy

Heavily n‐type doped and several nanometres thick In_0.485Ga_0.515P layers are necessary for various devices. We studied the delta‐doping of this ternary with tellurium; the layers were grown by metalorganic vapour phase epitaxy (MOVPE), and diethyltelluride was used as the precursor. A maximum Hall sheet concentration of 2.75 × 10¹³ cm^–2 was achieved in our samples grown at 560 °C. The Te profiles were analyzed with secondary ion mass spectrometry (SIMS), and a very narrow spectrum with a full width at half maximum of 7.5 nm was measured. This value indicates that the memory effect, referred to in the literature, was practically eliminated with appropriate growth conditions. (© 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Femtosecond laser micromachined optical waveguides in LiTaO3 crystal

By using femtosecond laser micromachining, optical wave guides in both depressed cladding and dual‐line configurations have been produced in LiTaO₃ crystal. The guiding properties and the thermal stability have been investigated for both geometries, which exhibit different performance. Depressed cladding waveguides support guidance along both extraordinary and ordinary index polarizations, while dual‐line waveguides support only extraordinary index polarization. Thermal annealing has been proved to be an effective method to reduce the propagation losses. For the cladding waveguide, the lowest propagation loss was as low as 0.38 dB/cm after the annealing treatment at 400 °C. (© 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X‐ray absorption study of the local structure at the NiO/oxide interfaces

This work reports an X‐ray absorption near‐edge structure (XANES) spectroscopy study at the Ni K‐edge in the early stages of growth of NiO on non‐ordered SiO₂, Al₂O₃ and MgO thin films substrates. Two different coverages of NiO on the substrates have been studied. The analysis of the XANES region shows that for high coverages (80 Eq‐ML) the spectra are similar to that of bulk NiO, being identical for all substrates. In contrast, for low coverages (1 Eq‐ML) the spectra differ from that of large coverages indicating that the local order around Ni is limited to the first two coordination shells. In addition, the results also suggest the formation of cross‐linking bonds Ni—O—M (M = Si, Al, Mg) at the interface.     

Pressure-induced structural transformations,orbital order and antiferromagnetism in La<Subscript>0.75</Subscript>Ca<Subscript>0.25</Subscript>MnO<Subscript>3</Subscript>

High pressure evolution of structural, vibrational and magnetic properties of La_0.75Ca_0.25MnO₃ was studied by means of X-ray diffraction and Raman spectroscopy up to 39 GPa, and neutron diffraction up to 7.5 GPa. The stability of different magnetic ground states, orbital configurations and structural modifications were investigated by LDA + U electronic structure calculations. A change of octahedral tilts corresponding to the transformation of orthorhombic crystal structure from the Pnma symmetry to the Immaone occurs above P ~ 6 GPa. At the same time, the evolution of the orthorhombic lattice distortion evidences an appearance of the e _g d _{x² ? z²} orbital polarization at high pressures. The magnetic order in La_0.75Ca_0.25MnO₃ undergoes a continuous transition from the ferromagnetic 3D metallic (FM) ground state to the A-type antiferromagnetic (AFM) state of assumedly 2D pseudo-metallic character under pressure, that starts at about 1 GPa and extends possibly to 20–30 GPa.     

Equation of state of planar hard dumbells

An extension of the hard disc equation of state to planar hard dumbells is proposed and the determination of the characteristic geometric measures of dumbells with the reduced length L* ? ?2 is discussed. The second and third virial coefficients following from the proposed equation of state are evaluated and compared with the exact Monte Carlo data. Compressibility factors for four different elongations are calculated and compared with pseudoexperimental data and with results of other methods.     

Crystallization and morphology in blends of isotactic polypropylene and linear polyethylene

Thermooptical, wide-angle x-ray diffraction and morphological investigations of blends of isotactic polypropylene with linear polyethylene revealed an increased crystallization rate of the polyethylene blend component, compared to crystallization of polyethylene alone. Crystallization behavior of the polyethylene component was markedly dependent on the blend thermal history and on the circumstances of the polyethylene phase—whether it was disperse or continuous. The higher crystallization rate of the polyethylene component was related to the presence of various types of heterogeneous crystallization nuclei in the blend and to the stabilizing action of the solid polypropylene matrix on minute polyethylene crystallites which survived above melting temperature.     

Time evolution of Wikipedia network ranking

X-ray circular magnetic dichroism, polarized neutron diffraction, ac susceptibility, and Seebeck effect have been measured for several members of the RCo₂ series (R = Ho, Tm, Er) as a function of temperature and applied magnetic field. The experimental results show robust parimagnetism (a general behaviour along the RCo₂ series with R being a heavy rare earth ion) and two reversal temperatures in some systems, which is an unexpected result. Polarised neutron diffraction show differences between results obtained on single crystals or polycrystalline ingots. We propose an interpretation of parimagnetic RCo₂ as a Griffiths phase of the high temperature, magnetically ordered, amorphous RCo₂ phase.