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The authors present here the superior result of synchrotron X-ray diffraction indexing of the 8 × 8 × 8 fluorite supercell, murataite, M8 (formula Ca66.37Mn29.33Ti186.76Zr83.35Al46.30Fe74.09O817, a = 39.277(3) Å, Z = 4). The authors present evidence that Fd$\bar 3$m (227) is the most likely space group.

We have used conventional X-ray powder diffraction to study one of the largest volume inorganic mixed oxide unit-supercell structures done so far. This necessitated some small-angle X-ray scattering-like observations at low angles from <2° 2θ to concord with electron diffraction, which had indicated an 8 × 8 × 8 huge volume supercell of a fluorite-type basic sub-cell. Emphasis is on the detection of, possibly very weak, fingerprint, low-angle/long lines/peaks which will indicate the (often unsuspected) presence of complex polytypic arrangements of simple very strong basic sub-cells and so facilitate future synthetic studies.

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Synchrotron X-ray powder diffraction pattern of the M8 murataite polytype

X-ray powder diffraction characterization of the large-volume unit cell of the M8 murataite polytype

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Synchrotron X-ray powder diffraction pattern of the M8 murataite polytype

X-ray powder diffraction characterization of the large-volume unit cell of the M8 murataite polytype