Lithium and Lead(II) Butyrates Binary System. Pure Compounds and an Intermediate Salt: From 2D to 3D Coordination Polymers
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The binary phase diagram between lithium and lead(II) butyrates, [xLiC3H7CO2 + (1 鈭?x)Pb(C3H7CO2)2] was determined by differential scanning calorimetry, in order to investigate the formation of intermediate salts. A complex or intermediate salt (with a 1:1 stoichiometry) was found during the solution of the phase diagram. Crystals of this salt, which melt incongruently at Tfus = 443.2 K, were obtained later by crystallization. The structures of the crystal phase of both pure compounds and the intermediate salt were solved by single crystal and powder X-ray diffraction, using synchrotron radiation. Lithium and lead(II) butyrates present a monoclinic unit cell (P21/c and P21/m, respectively). Both pure salts show a bilayered arrangement, in a structure of 2D coordination polymers, as usually metal alkanoates do. Nevertheless, the complex forms a microporous 3D ionic network (tetragonal, I41/a), very atypical in this kind of organic salts. Binary phase diagrams are proved to be a powerful tool to detect and predict the formation of intermediate crystals.

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