Hydrates and polymorphs of lead squarate Pb(C 4 O 4 ) Structural transformations studied by in situ X-ray powder diffraction and solid state NMR

Abstract : Considering the low dimensionality of the crystal structure of the known lead squarate tetrahydrate, Pb(C 4 O 4 )·4H 2 O, the thermal reactivity of the powdered compound and structural studies of lower hydrates have been investigated from X-ray single-crystal and powder diffraction data, solid state NMR and thermal analyses. It is shown that Pb(H 2 O)(C 4 O 4 ) and two polymorphs of anhydrous PbC 4 O 4 can be formed within different conditions. The departure of the water molecules leads to the condensation of initial inorganic chains into 2D or 3D-type crystal structures. The full decomposition of the squarate ligand provides successive lead oxides. © 2019 Elsevier Ltd
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T. Bataille, A. Bouhali, C. Kouvatas, C. Trifa, N. Audebrand, et al.. Hydrates and polymorphs of lead squarate Pb(C 4 O 4 ) Structural transformations studied by in situ X-ray powder diffraction and solid state NMR. Polyhedron, Elsevier, 2019, 164, pp.123-131. ⟨10.1016/j.poly.2019.02.047⟩. ⟨hal-02090016⟩

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