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Recently we carried out a series of photoinitiated reactions of zinc malonates with bis(pyridine-4-yl)ethylene. The transformation of {[Zn(bpe)(Me2mal)]xH2O}n to {[Zn(bpe)(Me2mal)]2[Zn2(tbcp)(Me2mal)]xH2O}n (Me2mal = dimethylmalonate, tpcb = tetrakis(pyridine-4-yl)cyclobutane) was proposed to be affected by dehydration reaction. Thus, we studied the effect of dehydration on above complex and its isostructural analog containing cyclobutane-1,1,-dicarboxylate. Both compounds were heated for 2 hours at 120 deg C until constant weight and then irradiated with UV for 8 hours. Transformations of crystalline compounds were controlled b means of powder diffraction and 1H NMR. Based on our data both compounds underwent a two-stage photoinitiated reaction.