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The metal organic layered structure catena-(bis(μ 2 -4,4'-bipyridine)-tris(μ 2 -oxalato)-bis(4,4'-bipyridine)-tri-zinc(ii)) ([Zn 3 (C 2 O 4 ) 3 (4,4'-bipy) 4 ]) was synthesized mechanochemically applying three different routes. The synthesis succeeded by i) simultaneously neat grinding the three starting materials zinc acetate dihydrate, oxalic acid dihydrate and 4,4'bipyridine, ii) grinding two compounds and adding the third afterwards, independent of the sequence. The products were characterized using powder X-ray diffraction, Raman spectroscopy, gas adsorption measurements, and scanning electron microscopy. Temperature-dependent synchrotron XRD measurements revealed that the monoclinic structure of [Zn 3 (C 2 O 4 ) 3 (4,4'-bipy) 4 ] rearranges reversibly to a higher ordered orthorhombic structure [Zn(C 2 O 4 )(4,4'-bipy)] at high temperatures.

Mechanochemical Synthesis of [Zn 3 (C 2 O 4 ) 3 (4,4'-bipy) 4 ] and its Reorganization at High Temperatures