Crystal structure, and the infrared and Raman spectra, of potassium, hydroxylamine-N,O-disulphonate, K2[O3SONHSO3]. The infrared and Raman spectra of potassium hydroxylaminetrisulphonate sesquihydrate, K3[O3SON(SO3)2]·1.5H2O

Abstract

The crystal structure of K₂[O₃SONHSO₃] has been determined using three-dimensional X-ray diffraction data with 1 097 observed reflections. Crystals are monoclinic, space group P2₁/a, with Z= 4 in a cell of dimensions a= 11.009(3), b= 10.040(2), c= 7.483(3)Å, and β= 109.49(2)°. The structure was solved by the heavy-atom method and refined by full-matrix least squares to R 0.033. The N–S bond [1.704(3)Å] is markedly longer than found for K₂[NH(SO₃)₂] in which both sulphonate groups are bound directly to nitrogen. The infrared (4 000–50 cm^–1) and Raman spectra of K₂[O₃SONHSO₃] and K₃[O₃SON(SO₃)₂]·1.5H₂O and their ¹⁵N and ²H derivatives at 77 K are reported and interpreted. Aqueous spectra have also been recorded. The following frequencies were assigned; ν(N–O), 925; ν(N–S), 808; and ν[S–O(N)], ca. 730 cm^–1 for K₂[O₃SONHSO₃]; ν(N–O), 930; ν_asym(N–S), 820; ν_sym(N–S), 757; and ν[S–O(N)], 708 cm^–1 for K₃[O₃SON(SO₃)₂]·1.5H₂O.