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Hermann Gies, M. Hochgräfe, B. Marler, C.A. Fyfe, Y. Feng, H. Grondey, G.T. Kokotailo
The structure of the low temperature (20K) form of zeolite ZSM-11 derived from 29Si MAS NMR spectroscopy, lattice energy minimization and Rietveld refinement
The crystal structure of the low temperature form of ZSM-11 (structure code MEL) was refined from high resolution synchrotron X-ray powder diffraction data, recorded at 20 K. Based on the results of 2D 29Si NMR investigations a model was obtained by energy minimization the Rietveld refinement of which converged in space group I 4 (No. 82) [a= 20.019(2)Å; c= 13.380(1)Å] to R1= 0.143 and Rwp= 0.126. Comparison of the theoretically predicted and experimentally determined structures against results from NMR experiments using the average T-T distance relationship between the structural parameters and the isotropic 29Si chemical shifts did not show any correlation with the results of the structure refinement. However, with the values obtained from the energy-minimized structure model a good correlation between the structural parameters and the chemical shifts of Si was obtained for one of the two possible assignments of the NMR chemical shifts to Si-sites. The fit of the energy minimized model to the experimental data set gave R1= 0.179 and Rwp= 0.157. Since the NMR experiment gives direct information about the local ordering and structural state of the material this demonstrates the potential of the modeling experiment and also reveals the limits in accuracy and precision of the Rietveld structure refinement.
Zeitschrift für Kristallographie, Oldenbourg Wissenschaftsverlag
Print ISSN: 0044-2968
Volume: 211, 04/1996
Pages: 221