Nitrosodisulfonates and hydroxylamine-N,N-disulfonates.  II.  Crystal structure of a rubidium hydroxylamine-N,N-disulfonate

Guttormson, R. J.; Rütherford, J. S.; Robertson, B. E.; Russell, David

doi:10.1021/ic50139a004

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“…Previous articles in this series (1)(2)(3) have discussed the preparation and characterisation of a number of alkali metal salts of hydroxylamine-N,N-disulphonate and related ions, and have examined the epr spectra of these salts when irradiated to compare the spectra obtained with the spectra obtained from Fremy's salt, both as a pure solid, when a triplet state species is observed (2,4), and as a dilute solid solution in the corresponding potassium hydroxylamine-N,N-disulphonate, when a free radical species is observed (5). In particular, the triplet state epr 'Author to whom correspondence may be addressed.…”

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confidence: 98%

Nitrosodisulphonates and hydroxylamine-N,N-disulphonates. V. A potassium salt of hydroxylamine-N,N-disulphonic acid with a displacive superlattice structure

Rütherford¹,

Robertson²,

Guttormson³

et al. 1988

Can. J. Chem.

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and hydroxylamine-N,N-disulphonates. V. A potassium salt of hydroxylamine-N,N-disulphonic acid with a displacive superlattice structure. Can. J. Chem. 66, 655 (1988).The structure of the potassium salt of hydroxylamine-N,N-disulphonate, with the formula KsHN2S40a14.H20, has been determined by X-ray diffraction. The crystals are triclinic, a = 14.01 1 (6), b = 16.1 18(9), c = 1 1.867(6) A. a = 103.28(6), p = 106.76(3), y = 86.38(3)", PI with Z = 6. The integrated intensities of 8694 independent reflections were measured on a four-circle diffractometer, 5236 of which were used in the refinement to give a final least-squares weighted residual of 0.107 and a conventional R factor of 0.081.The structure forms a six-fold derivative lattice, which arises by small displacements (ca. 0.2 A) of the atom ositions from an average structure which is triclinic with Z = 1. This results in three very short H bonds, average length 2.46 1 , which link the three independent anion-dimers, being symmetry-free in this structure. Other bond lengths and angles in the anions are very similar to those in the Rb salt. The K' ions show 8 , 9 , and I0 coordination, in a number of different polyhedral types. The three independent water molecules are each coordinated to three totally distinct K+ ions, and are linked to the anions by weak H bonds. The structural complexity 'may be explained in terms of a Lewis acid-base "mismatch" of the cations and anions present.

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