High‐pressure Raman spectroscopic and other structural studies of hydrotalcites containing intercalated dicarboxylic acid anions

Abstract

The results of pressure-tuning Raman spectroscopic, X-ray powder diffraction and solid-state 13 C-NMR studies of selected dicarboxylate anions intercalated in a Mg-Al layered double hydroxide lattice are reported. The pressure dependences of the vibrational modes are linear for pressures up to 4.6 GPa, indicating that no phase transitions occur. The interlayer spacings show that the oxalate, malonate and succinate dianions are oriented perpendicular to the layers, but the glutarate and adipate are tilted. The solid-state 13 C-NMR spectra of these materials show full chemical shift anisotropy and, therefore, the anions are not mobile at room temperature.

Solid state NMR studies of layered double hydroxides

“…SSNMR is generally used as one of several techniques for structural characterization of LDH intercalated with organic molecules, where δiso( 13 C) obtained from δiso( 13 C) CP MAS NMR is used to fingerprint studies including UV-filters [48], surfactants [133], small dicarboxylic acids [134], biand tricycling carboxylates [135], metalorganic molybdenum [136] and Pd(II) complexes [137],…”

Recent advances in linear and nonlinear Raman spectroscopy. Part VI

“…Zhu and Pezzotti carried out a theoretical Raman polarization analysis for the corundum structure of sapphire (Al 2 O 3 ) and conducted validation experiments for the purpose of retrieving the full set of phonon deformation potentials . Wright and co‐workers reported the results of high‐pressure Raman spectroscopic and other structural studies of hydrotalcites containing intercalated dicarboxylic acid anions …”