The results of in situ synchrotron X-ray powder diffraction experiments conducted during the synthesis of iron-deficient Na+/H3O+ and K+/H3O+ jarosites at temperatures in the range 80 to 120 °C are presented. They demonstrate that samples can be prepared in which the iron-site vacancies are ordered. The ordering is accompanied by a lowering of symmetry, from rhombohedral, space group Rm, to monoclinic, C2/m. The implications for magnetic properties are discussed.

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