Because electron diffraction can sample individual microcrystals, it is clear that this single crystal method can facilitate, in at least two ways, structure determination for inorganic materials, such as zeolites, that are preferentially microcrystalline. First, in a qualitative application, three-dimensional tilts of individual small crystals, to map the reciprocal lattice, greatly facilitates unit cell and space group determination when powder diffraction indexing programs fail. If incoherent multiple scattering leads to violation of systematic absences, these absences can be restored by collection of precession diffraction patterns based on the Vincent-Midgley method [1], as demonstrated recently [2]. The second, quantitative application, i. e. ab initio structure determination from electron diffraction intensity data, also seems to be feasible. In the auspicious case of thin layered zeolite crystals in the MWW framework, the three-dimensional structure was determined by direct methods based on maximum entropy and likelihood [3], the only difficulty arising from the ’missing cone’ of structural information imposed by the goniometric tilt limit. Possible methods for restoration of the missing information, although approximately provided by phase and amplitude prediction (Sayre equation), include alternate crystallization of the desired crystal projection by appropriate structure directing agents, or, simply, by sectioning the desired view of the structure in available samples. Multiple scattering perturbations include both n-beam dynamical and secondary scattering; collection of precession data greatly reduces the latter influence [2], facilitating ab initio analyses via direct methods (e. g. tests on LTA, ITQ-1, ITQ-7, ZSM-10, MOR, MCM-68), while systematic dynamical diffraction is still observed (even at 300 kV). Improved collection of intensity data via imaging plates, exploiting a much greater linear response to intensity, is also recommended. One other, largely unexplored, possibility is to collect zero loss electron diffraction intensities in electron microscopes with in-line ’omega’ energy filters. Generally, for unknown zeolite structures, electron diffraction analyses have been carried out in parallel with the usual powder determinations, not only to provide needed symmetry information but also to detect structural details of important zones, e. g. the location of porous channels to guide the powder determination; in some cases, the crystal structure would not have been solved without this electron crystallographic information. Whether or not true ab initio electron crystallography can ever exist as an independent structural tool for zeolites remains a question to be answered by ongoing research.
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