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K 4 [Fe(CN) 5 NO 2 ]⋅KNO 2 ⋅H 2 O crystallizes in the non-centrosymmetric orthorhombic space group  Bb 2 1  m  (no. 36) with  a  = 2698.2(3),  b  = 1415.7(1),  c  = 849.6(1) pm and Z = 8 at 291 K. Due to a high degree of pseudosymmetry the deviations from centrosymmetry are small. The gross arrangement of the iron and potassium atoms is that of the AlB 2 -type, discernible from the distorted hexagons of the boron-analogous part with the composition FeK 3  while further potassium atoms are replacing Al in agreement with the formulation K 2 [FeK 3 ]. The disorder of the free nitrite ions affiliated to KNO 2  is characterized by means of additional data sets collected at temperatures of 173 K and 363 K. The results of the structure analysis are confirmed by infra-red spectroscopy. Especially the deformation modes  δ (O-N-O) of the free nitrite and those of the nitro ligand show the expected frequency splitting. Mössbauer data serve as a check on chemical composition and give an independent estimate for the mean square displacement of the iron ( 57 Fe) atoms comparable to the results from X-ray diffraction. The loss of crystal water above 400 K is registered using ther-mogravimetry and differential scanning calorimetry.

Crystal structure analysis, pseudosymmetry and spectroscopic data of K 4 [Fe(CN) 5 NO 2 ]⋅KNO 2 ⋅H 2 O