Premium
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
Author(s) -
Bahemmat Samira,
Neumüller Bernhard,
Ghassemzadeh Mitra
Publication year - 2015
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201500255
Subject(s) - chemistry , thermal decomposition , acetylacetone , coordination polymer , copper , inorganic chemistry , cyclic voltammetry , differential thermal analysis , polymer chemistry , oxalic acid , thermal stability , coordination complex , thermogravimetric analysis , nuclear chemistry , electrochemistry , crystal structure , crystallography , organic chemistry , metal , physics , electrode , diffraction , optics
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.