Benzophenone was the first organic molecular material to be identified as polymorphic. It is well known that benzophenone crystallizes in a stable orthorhombic alpha-form (m.p. 321 K) with space group P2(1)2(1)2(1) and a = 10.28, b = 12.12, c = 7.99 A, [Girdwood (1998). Ph.D. thesis. Strathclyde University, Glasgow, Scotland]. Here we report two separate structure determinations of the metastable beta-form (m.p. 297-299 K). Crystalline material of the metastable polymorph was obtained from a melt supercooled to approximately 243 K. The structure was determined from X-ray powder diffraction data by employing a novel, computational systematic search procedure to identify trial packing arrangements for subsequent refinement. Unit-cell and space-group information, determined from indexing the powder diffraction data, was used to define the search space. The structure was also determined from single-crystal diffraction data at room temperature and at 223 K. The metastable phase is monoclinic with space group C2/c and a = 16.22, b = 8.15, c = 16.33 A, beta = 112.91 degrees (at 223 K). The structures derived from the individual techniques are qualitatively the same. They are compared both with each other and with the stable polymorph and other benzophenone derivatives.
The Oseberg collection includes the most complete ensemble of wooden remains from the Viking Age. However, since many of the wooden objects were treated with alum in the early 1900s, they now suffer from dramatic conservation issues. A multi-analytical approach was adopted to investigate both the organic and the inorganic components of some selected wood fragments, with the aim of fully characterising the materials and their decomposition products. A particular focus was taken on the differences between the surface and the core of the fragments analysed, and on the correlations between the results obtained by the different techniques, in order to disclose possible interactions between the materials during degradation. In addition to differences in alum concentration and wood alteration between the surface and the core, some decomposition/transformation products of alum, such as mercallite (KHSO4), were identified by FTIR and XRD. Contextual interpretation of the results obtained by ICP-OES elemental analysis of inorganic components and Py(HMDS)-GC/MS characterisation of degraded lignocellulosic materials supported some previous observations about potential relationships between specific metals (Al, Fe, Ca) and wood degradation and enabled new correlations to be highlighted. Although similar degradation patterns were revealed in the investigated objects–depletion of holocellulose, oxidation of lignin and some transformation of alum - a notable variability at the molecular level was highlighted. This is an important factor to be taken into account for the planning of re-treatment strategies of these extremely precious artefacts
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