The efficacy of direct methods for solving the crystal structures of zeolites from electron diffraction data is evaluated for a series of related materials, i.e. MCM-22, MCM-49 and ITQ-1. First, it is established by tilting experiments that all materials share the same MWW framework. The calcined product of a delaminated MCM-22 precursor, ITQ-2, also shares this framework structure within the limited number of stacked unit cells. For all materials, the underlying space group is P6/mmm where a [asymptotically equal to] 14.21, c [asymptotically equal to] 24.94 A. Traditional direct methods are useful for determining the projected structure down the hexagonal axis but are not very effective for finding the three-dimensional structure. On the other hand, maximum-entropy and likelihood approaches are effective for determining either 2D projections or 3D frameworks. The major restriction to 3D determinations by direct methods is the limited goniometric tilt range of the electron microscope, hence the `missing cone' of information. Potential maps from the most accurate phase sets are, therefore, observed as continuous density envelopes to the true structure. Some improvement is found when the Sayre equation predicts missing amplitudes and phases but it is clear that better specimen preparation methods are required to include projections containing the c* axis of the reciprocal lattice.
Dorset, D. L., Roth, W. J., & Gilmore, C. J. (2005). Electron crystallography of zeolites - The MWW family as a test of direct 3D structure determination. Acta Crystallographica Section A: Foundations of Crystallography, 61(5), 516–527. https://doi.org/10.1107/S0108767305024670