The title compound, (NH 4 ) 2 [FeCl 5 H 2 O] has been prepared by reaction between iron(III) chloride and ammonium chloride which was formed by hydrolysis of isonicotinamide or thionicotinamide in ethanol. The characterization was based on elemental analysis and infrared spectra. The crystal structure of the title compound has been refi ned by single crystal X-ray diffraction method at 293 K. Crystals are orthorhombic, Pnma, with unit cell parameters: a = 13.760(1) Å, b = 9.960(1) Å, c = 7.060(1) Å, Z = 4 and R = 3.5 %. The iron(III) atom in [FeCl 5 2-ion is approximately octahedrally coordinated by fi ve Cl atoms and one O atom of H 2 O molecule. This distortion is caused by the extensively hydrogen-bonded lattice. Structural parameters and IR spectra of similar compounds are compared and discussed.
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