Synchrotron radiation X-ray diffraction and Raman spectroscopy study of l-asparagine monohydrate doped with Fe(III) at high pressure.

Crystals of l-asparagine monohydrate doped with Fe(III) were studied by Raman spectroscopy in a diamond anvil cell (DAC) in the spectral range from 100 to 3200 cm-1 and pressures up to 9.2 GPa. The behavior of external modes suggests conformational changes between 3.0 and 4.0 GPa mainly affecting the CH2 group. X-ray diffraction measurements with synchrotron radiation were performed in the angular range from 3 to 12 degrees (2θ) up to 9.3 GPa. The lattice parameters contract up to 9.3 GPa, with the exception of parameter b, which exhibits expansion from 7.2 GPa. The lattice parameters exhibit discontinuities between 3.0 and 4.0 GPa, this effect is compatible with conformational changes. Such modifications occur without a change in symmetry, at least up to 9.3 GPa. Under decompression, down to atmospheric pressure, the original Raman spectrum is recovered, showing that the conformational change and the other changes are all reversible.

Pressure-induced phase transitions in MBANP crystal: A study by synchrotron radiation X-ray diffraction and Raman spectroscopy.

Raman spectroscopy and synchrotron radiation X-ray diffraction have been used to study the effect of pressure on 2-(-α-methylbenzylamino)-5-dinitropyridine (MBANP). Several changes are observed with increasing pressure in the Raman spectra of this system, such as splitting of various bands and disappearance of bands. Discontinuous shifts in wavenumber vs pressure plot indicate that a conformational phase transition takes place around 0.5 GPa. The behavior of the Raman spectra indicates that MBANP molecules present conformational phase transition at high-pressure. X-ray diffraction, performed with synchrotron radiation, confirms the conformational changes observed by Raman experiments around 0.5 GPa. The pressure provokes a rotational movement of the benzene ring which can be associated with the conformational phase transition.

Low-temperature Raman spectra of the 2-(α-methylbenzylamino)-5-nitropyridine crystal.

The polar organic 2-(α-methylbenzylamino)-5-nitropyridine crystal (MBANP) has been studied by Raman spectroscopy at low temperatures (from 300 to 10K). The effect of temperature change on the vibrational spectrum is discussed with the aid of DFT calculations. The behavior of the Raman spectra indicates that MBANP molecules present a different conformation at low temperatures associated with the rotation of the phenyl and pyridine rings. Temperature-dependent X-ray measurements and differential scanning calorimetry (DSC) analysis were utilized as complementary techniques to investigate the structural stability of MBANP crystal.