Comment to 13C-NMR studies of alpha and gamma polymorphs of glycine.

Glycine provided to research laboratories by chemical companies can contain different polymorphs and/or mixture of polymorphs. The alpha- and gamma-glycine differ slightly in 13C shielding parameters and very much in dynamic properties. The isotropic values of chemical shifts for carboxyl groups of alpha- and gamma-glycine are found to be delta(iso) = 176.50 ppm and delta(iso) = 174.60 ppm, respectively. By using cross-polarization contact time equal to 20 ms, the intensity of carboxyl signal arising from gamma-glycine is reduced almost to zero, while that of alpha-glycine is only slightly depleted compared to the intensity of signal recorded at contact time of 1 ms. In contrast, for alpha-form, the 13C T1 relaxation time of carboxyl carbon is five times shorter compared to gamma-form.

Refinement of framework disorder in dehydrated CaA zeolite from single-crystal synchrotron data.

An accurate knowledge of zeolite structure is required for understanding their selective sorption capacities and their catalytic properties. In particular, the positions of the exchangeable cations and their interactions with the framework are essential. The present study deals with the accurate crystal structure determination of a fully exchanged and fully dehydrated CaA zeolite (Ca(48)Al(96)Si(96)O(384), Fm3c, a = 24.47 A) using single-crystal high-resolution synchrotron X-ray diffraction [(sin straight theta/lambda)(max) = 1.4 A(-1)]. It is shown that cation exchange severely distorts the skeleton, especially around the O2 atom. The high-resolution synchrotron data reveal that this latter O atom is disordered and lies out of the mirror plane it occupies in other A-type zeolites. This feature is related to that observed for Ca(2+) cations.