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

• Published in: European journal of inorganic chemistry Vol. 2015; no. 24; pp. 4116 - 4124
• Main Authors: Bahemmat, Samira, Neumüller, Bernhard, Ghassemzadeh, Mitra
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.08.2015; WILEY‐VCH Verlag; Wiley Subscription Services, Inc
• Subjects: Coordination modes; Coordination polymers; Copper; Nanosheets; Nanostructures; Thermolysis
• ISSN: 1434-1948; 1099-0682
• DOI: 10.1002/ejic.201500255

The synthesis, characterization, and thermal decomposition behaviour of the oxalato‐bridged copper(II) coordination polymer [Cu2(C2O4)(L)2Cl2(MeOH)2]n (1) (L = 3,5‐dimethyl‐1H‐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. The one‐pot reaction of acetylacetone, thiosemicarbazide, oxalic acid and copper(II) chloride in a molar ratio of 2:2:1:2 affords coordination polymer [Cu2(C2O4)(L)2Cl2(MeOH)2]n (1) (L = 3,5‐dimethyl‐1H‐pyrazole generated in situ). Thermolysis of complex 1 under neat conditions in air at 550 °C and 1000 °C generates CuO nanoparticles and nanosheets, respectively.