One‐Pot Synthesis of an Oxalato‐Bridged Cu II Coordination Polymer Containing an In Situ Produced Pyrazole Moiety: A Precursor for the Preparation of CuO Nanostructures

The synthesis, characterization, and thermal decomposition behaviour of the oxalato‐bridged copper(II) coordination polymer [Cu 2 (C 2 O 4 )(L) 2 Cl 2 (MeOH) 2 ] n ( 1 ) (L = 3,5‐dimethyl‐1 H ‐pyrazole) is reported. Complex 1 is prepared in a straightforward fashion by a one‐pot reaction of acetylacetone, thiosemicarbazide, oxalic acid and copper(II) chloride in a molar ratio of 2:2:1:2. Complex 1 was characterized by means of FT‐IR spectroscopy, mass spectrometry and elemental analysis as well as single‐crystal X‐ray diffraction. Furthermore, the electrochemical behavior of 1 was investigated in DMSO by cyclic voltammetry. The thermal stability of complex 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Solventless thermolysis of complex 1 at 550 °C and 1000 °C under air afforded copper oxide nanoparticles and nanosheets, respectively. The CuO nanostructures were characterized by using a series of techniques including FT‐IR, UV/Vis, XRD, XPS, EDAX, and SEM.