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Synthesis and Characterization of Heterocyclic Substituted Pentacyanoferrate (II) Complexes: UV-Visible, Infrared, Mossbauer, TGA-DTG and XRD

A series of substituted compounds Na3[Fe(CN)5L]nxH2O where L= nicotinic acid, nicotinamide, 2,3,4-cyanopyridine and isonicotinamide have been synthesized. These pentacyanoferrates complexes studies by UV-visible, infrared, Mössbauer spectroscopic, TGA-DTG and XRD. All complexes has an absorption band in the visible region that is assigned to d-d transition. The Mössbauer spectra of these pentacyanoferrates complexes exhibit quadrupole doublet ΔEQ=0.71-084 mms -1 at room temperature. The isomer shift (δ) values fall within 0.00 ± 0.02 mms -1 suggest the iron atom in +2 low spin states. The complex start decomposing at 60 o C yielding residual weight 17.0-20.1. The Mössbauer spectra at higher temperatures and TGA/DTG of the complexes show that solids yielding into metal carbides, magnetite (F3O4(A) and F3O4(B) and hematite (F2O3). Mössbauer spectra recorded after heating at 150, 200, 250 and 300 o C exhibit symmetric doublet suggested partial decomposition. At 500 o C, a six line pattern starts appearing which on further heating at > 700 o C turns into eight or ten lines suggesting the formation of Fe3O4(A), Fe3O4(B) of different particle sizes and iron carbide Fe3C along with metal phase. The XRD powder pattern of the 2,3,4-cyanopyridine substituted pentacyanoferrate complexes after heating at 950 o C showed an intense lines corresponds to the formation of γ-