differential thermal analysis
Wiley InterScience Backfile Collection 1832-2000
Chemistry and Pharmacology
Mixtures of N2O3 and N2O4 have been prepared from measured volumes of NO and O2. Phase relationships in the system N2O3/N2O4, which depend on the composition of the samples and on the temperature, were studied by the Guinier technique and differential thermal analysis. Single crystals of phases A and B of N2O3 were grown in situ on a diffractometer and studied at temperatures between -107 and -170°C by X-ray diffraction. The structure analysis of A-N2O3 (tetragonal, space group I41/a, T = -170°C, a = 1625.57 (16), c = 880.49(13) pm, Z = 32, R1 = 0.051 for 1030 unique reflections) is hampered by twinning and additional disorder of one of two crystallographically independent molecules. B-N2O3 is nicely ordered with one molecule in the asymmetric unit (orthorhombic, space group P212121, T = -160°C, a = 506.86(4), b = 647.96(5), c = 863.26(6) pm, Z = 4, R1 = 0.023 for 1352 unique reflections). The most interesting features of the N2O3 molecule are its planarity and the extraordinarily long N—N bond (189.0(1) pm).
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