Polymorphisme du dioxotriplomb (II) tetraoxosulfate (VI) Pb3O2(SO4) a basse temperature. II - Etude structurale de la phase ferroelastique gamma-Pb3O2 (SO4) par diffraction neutronique sur poudres a 2 et 45K

Full-profile neutron powder diffraction structure refinements of dioxotrilead(II)tetraoxosulfate(VI) at 2 and 45K reveal that both the alpha- and the gamma-Pb₃O₂ (SO₄) polymorphs have to be refined simultaneously at these temperatures. Accordingly, the paraelastic alpha phase is trapped in the ferroelastic gamma phase, yielding thus mixtures of both compounds in a nearly 1:1 molar ratio. Both structures are essentially similar. The slight variations of the lead-oxygen distances in the infinite edge-sharing tetrahedral (Pb₃ O₂)n double-chains force the sulfate group to adopt nearly C3v and C2v site symmetries respectively in the alpha and gamma phases. The present work is a good example of the behaviour of the DBW3.2 program (1) when mixtures of very similar structures are refined simultaneously (high correlation between some structural parameters).