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Studies on a "Disappearing Polymorph": Thermal and magnetic characterization of α-p-NCC6F4CNSSN•

AuthorsArauzo, Ana B.; Palacio, Fernando; Rawson, Jeremy M.
Issue Date2016
PublisherAmerican Chemical Society
CitationJournal of the American Chemical Society 138: 16779-16786 (2016)
AbstractThe α-and β-phases of the thiazyl radical p-NCCFCNSSN (1) can be selectively prepared by careful control of the sublimation conditions, with the α-phase crystallizing preferentially when the substrate temperature is maintained below −10 °C, whereas the β-phase is isolated when the substrate temperature is maintained at or above ambient temperature. Differential scanning calorimatry studies reveal that the α-phase converts to the β-phase upon warming over the range 111-117 °C (ΔH = +4 kJ·mol) via a melt-recrystallization process, with the β-phase itself melting at 167-170 °C (ΔH = 27 kJ·mol). IR and Raman spectroscopy can be used to clearly discriminate between 1α and 1β. The α-phase shows a broad maximum in the magnetic susceptibility around 8 K that, coupled with a broad maximum in the heat capacity, is indicative of short-range order. Some field dependence of the susceptibility below 3 K is observed, but the lack of features in the ac susceptibility, M vs H plots, or heat capacity mitigates against long-range order in 1α.
Identifiersdoi: 10.1021/jacs.6b10707
e-issn: 1520-5126
issn: 0002-7863
Appears in Collections:(ICMA) Artículos
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