@article {1115,
	title = {Solid state NMR method for the determination of 3D zeolite framework/sorbate structures: H-1/Si-29 CP MAS NMR study of the high-loaded form of p-xylene in ZSM-5 and determination of the unknown structure of the low-loaded form},
	journal = {Journal of the American Chemical Society},
	volume = {127},
	number = {20},
	year = {2005},
	note = {ISI Document Delivery No.: 928AXTimes Cited: 22Cited Reference Count: 57},
	month = {May},
	pages = {7543-7558},
	type = {Article},
	abstract = {A general protocol is described for structure determinations of organic sorbate-zeolite complexes based on the selective, through-space, distance-dependent transfer of magnetization from protons in selectively deuterated organics to framework silicon nuclei. The method was developed using the known structure of the high-loaded ZSM-5/p-xylene complex containing p-xylene-d(6) or p-xylene-d(4). It was then applied to determine the unknown structure of the low-loaded ZSM-5/p-xylene complex using NMR alone. For the high-loaded complex improved data were obtained below 273 K, where slow motions and exchange processes of the p-xylene are eliminated. The general approach was validated by. the exact agreement of the experimental H-1-Si-29 CPMAS spectra obtained at a specific contact time and the complete 24-line spectra simulated using 1/T-CP vs M-2 correlations from only the six clearly resolved resonances. For the low-loaded complex the Si-29 resonances were assigned at 267 K, and variable contact time CP experiments were carried out between 243 and 173 K using the same specifically deuterated p-xylenes. All possible locations and orientations of the p-xylene guests were sampled, and those solutions that gave acceptable linear 1/T-CP vs M-2 correlations were selected. The optimum p-xylene location in this temperature range was determined to be in the channel intersection with the long molecular axis parallel to [0,1,0] (ring center fractional coordinates {-0.009, 0.250, 0.541}) with the ring plane oriented at an angle of 30 +/- 3 degrees about the crystallographic b axis. A subsequent single-crystal X-ray study confirmed this predicted structure.},
	keywords = {3-DIMENSIONAL BONDING CONNECTIVITIES, CROSS-POLARIZATION, CRYSTAL STRUCTURE-ANALYSIS, LATTICE, MAGIC-ANGLE, NATURAL-ABUNDANCE, NUCLEAR-MAGNETIC-RESONANCE, PROTON-ENHANCED NMR, SINGLE-CRYSTAL, SPINNING NMR, structures},
	isbn = {0002-7863},
	url = {<Go to ISI>://000229244600061},
	author = {Fyfe, C. A. and Diaz, A. C. and Grondey, H. and Lewis, A. R. and Forster, H.}
}
@article {5080,
	title = {Location of the fluoride ion in tetrapropylammonium fluoride silicalite-1 determined by H-1/F-19/Si-29 triple resonance CP, REDOR, and TEDOR NMR experiments},
	journal = {Journal of the American Chemical Society},
	volume = {123},
	number = {28},
	year = {2001},
	note = {ISI Document Delivery No.: 451LFTimes Cited: 48Cited Reference Count: 50},
	month = {Jul},
	pages = {6882-6891},
	type = {Article},
	abstract = {The location of the fluoride ion in tetrapropylammonium fluoride silicalite-1 ([TPA]-F-[Si-MFI]), an as-synthesized siliceous zeolite with the MEI topology, has been unambiguously determined using solid-state NMR experiments alone. With the H-1 {\textendash}> Si-29 CP-INADEQUATE experiment, the 12 peaks in the highly resolved Si-29 MAS NMR spectrum of [TPA]-F-[Si-MFI] were assigned. Using these peak assignments it was possible to perform H-1/F-19/Si-29 triple resonance CP, REDOR, and TEDOR experiments to measure F-Si distances and thus locate the fluoride ion. It is covalently bonded to Si-9 in the [4(1)5(2)6(2)] cage of the zeolite framework and exchanges between two "mirror-related" Si-9 sites, making them equivalent on the NMR time scale. The importance of this result and the general applicability of the approach are discussed.},
	keywords = {3-DIMENSIONAL BONDING CONNECTIVITIES, 5-COORDINATE, CONTAINING OCTADECASIL, CROSS-POLARIZATION NMR, CRYSTAL-STRUCTURE, DETERMINATIONS, DISTANCE, MAS-NMR, NATURAL-ABUNDANCE, PROTON-ENHANCED NMR, SILICON, SOLID-STATE SI-29},
	isbn = {0002-7863},
	url = {<Go to ISI>://000169803000018},
	author = {Fyfe, C. A. and Brouwer, D. H. and Lewis, A. R. and Chezeau, J. M.}
}
@article {3696,
	title = {The structure of the low temperature (20 K) form of zeolite ZSM-11 derived from Si-29 MAS NMR spectroscopy, lattice energy minimization and Rietveld refinement},
	journal = {Zeitschrift Fur Kristallographie},
	volume = {211},
	number = {4},
	year = {1996},
	note = {ISI Document Delivery No.: UG444Times Cited: 8Cited Reference Count: 17},
	pages = {221-227},
	type = {Article},
	abstract = {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 Si-29 NMR investigations a model was obtained by energy minimization the Rietveld refinement of which converged in space group <I(4)over bar> (No. 82) [a = 20.019(2) Angstrom; c = 13.380(1) Angstrom] to R(I) = 0.143 and R(wp) = 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 Si-29 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 chemicals 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 R(I) = 0.179 and R(wp) = 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.},
	keywords = {beta, COMBINATION, CONNECTIVITIES, lattice energy minimization, NATURAL-ABUNDANCE, Rietveld refinement, Si-29 NMR, SOLID-STATE NMR, X-RAY-DIFFRACTION, zeolites},
	isbn = {0044-2968},
	url = {<Go to ISI>://A1996UG44400001},
	author = {Hochgrafe, M. and Marler, B. and Gies, H. and Fyfe, C. A. and Feng, Y. and Grondey, H. and Kokotailo, G. T.}
}
@inbook {3334,
	title = {One and two-dimensional solid-state NMR investigations of the three-dimensional structures of zeolite-organic sorbate complexes},
	booktitle = {Zeolites: A Refined Tool for Designing Catalytic Sites},
	series = {Studies in Surface Science and Catalysis},
	volume = {97},
	year = {1995},
	note = {ISI Document Delivery No.: BE46VTimes Cited: 2Cited Reference Count: 25Proceedings PaperInternational Zeolite SymposiumOCT 15-20, 1995QUEBEC CITY, CANADASARA BURGERHARTSTRAAT 25, PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS},
	pages = {1-10},
	publisher = {Elsevier Science Publ B V},
	organization = {Elsevier Science Publ B V},
	address = {Amsterdam},
	keywords = {3-DIMENSIONAL BONDING CONNECTIVITIES, FORM, LATTICE, NATURAL-ABUNDANCE, PARA-XYLENE, TEMPERATURE, ZSM-5},
	isbn = {0-444-82130-9},
	url = {<Go to ISI>://A1995BE46V00001},
	author = {Fyfe, C. A. and Grondey, H. and Diaz, A. C. and Kokotailo, G. T. and Feng, Y. and Huang, Y. and Wongmoon, K. C. and Mueller, K. T. and Strobl, H. and Lewis, A. R.},
	editor = {Bonneviot, L. and Kaliaguine, S.}
}
