Crystal Research and Technology
Cryst. Res. Technol. 40, 212 (2005) - Abstract -

Synthesis and characterization of (NH4)2CuBr2Cl2.2H2O crystals

G. Amirthaganesan, M. A. Kandhaswamy, and V. Srinivasan

Department of Chemistry, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore – 641 020, India

Keywords single crystals, thermogravimetry, phase transitions, Differential Scanning Calorimetry
PACS 61.10Nz, 33.20.Ea, 81.10.Dn, 81.70.Pg
DOI 10.1002/crat.200410327

Single crystals of a new compound, (NH4)2CuBr2Cl2.2H2O, were grown from saturated aqueous solution at room temperature by slow evaporation method. The grown crystals were characterized through elemental, powder XRD, thermal and DSC analyses and FTIR and far IR spectra. The elemental analysis and the decomposition pattern formulated using the TG-DTG studies confirm the stoichiometry of the compound. The crystallinity of the compound is confirmed from the powder XRD pattern. A preliminary single crystal X-ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with a = 7.7466Å, b = 7.783Å and c = 8.1211Å. The low temperature DSC shows thermal anomalies at –161.1, 156.5, –152.4, –145.2, –134, -18.5, and 1.4°C during the heating run and at –4.3, -54.8, -66.1, -90.6, -109.7 and –147.2°C during the cooling run. The thermal hysterses indicate first order phase transitions in the title compound at these temperatures. The FTIR spectra were used to assign the characteristic vibrational frequencies due to NH4+, CuX42- ions and other chemical bonds. The effect of substitution of two bromine atoms on the phase transitions of a closely related crystal, diammonium tetrachloro cuprate dihydrate is also discussed.





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