XRD, FE-SEM, FT-IR and ESR studies of cation deficient potassium tris(oxalato)ferrate(III)trihydrate

Cation deficient potassium tris(oxalato)ferrate(III)trihydrate {K_2.72[Fe(C₂O₄)₃]·3.17H₂O} crystals were characterized by X-ray powder diffractogram, Fourier Transform Infrared Spectroscopy (FT-IR), quantitative elemental analysis of EDAX, Field Emission Scanning Electron Microscope (FE-SEM), Electron Spin Resonance Spectroscopy (ESR) and Thermogravimetry And Diffrential thermal analysis (TG-DTA). This compound crystallizes in the monoclinic system with P2₁/c space group and shows three-dimensional (3D) chain structure. The elements present in the grown crystal were confirmed by the energy dispersive X-ray analysis (EDAX). The microstructural features on the surface of the single crystals were determined using FE-SEM. Powder X-ray diffraction results indicate the polycrystalline nature of the material. Infrared spectroscopy was used to study the vibrational modes of the compound. The room temperature crystalline ESR spectra indicate the high-spin (S = 5/2) of Fe(III) ion. Thermal behaviour of the compound has been studied using thermogravimetry and diffrential thermal analysis. (paper)