We use cookies to ensure that we give you the best experience on our website. By continuing to browse this repository, you give consent for essential cookies to be used. You can read more about our Privacy and Cookie Policy.

Durham e-Theses
You are in:

Combined use of powder diffraction and magic-angle spinning NMR to structural chemistry

King, Ian James (2003) Combined use of powder diffraction and magic-angle spinning NMR to structural chemistry. Doctoral thesis, Durham University.

[img]Archive (ZIP) (Topas input file for the structure of ZrP2O7 and .cif and .lst file for 2-[4-(2-hydroxy-ethylamino)-6-phenylamino-[1,3,5]triazin-2-ylamino]-ethanol) - Supplemental Material


A range of 1D and 2D MAS NMR experiments have been carried out in conjunction with X-ray diffraction experiments on a number of materials from the AM(_2)O(_7) family, which exhibit the unusual phenomenon of negative thermal expansion. It has been shown that ZrP(_2)O(_7) and HfP(_2)O(_7) exist with space group Pbca rather than Pa3 as proposed in the literature, and a full structure solution has been possible for ZrP(_2)O(_7) from a combination of NMR and X-ray and neutron powder diffraction. 2D MAS NMR has been used to differentiate at least 108 unique phosphorus sites within the asymmetric unit of SnP(_2)O(_7), supporting a recent powder diffraction study presented in the literature. PbP(_2)O(_7) has been shown, by NMR, to exist as an incommensurate phase at room temperature. ZrW(_2)O(_8), a material which also shows negative thermal expansion, has been studied here primarily with variable-temperature (^17)O MAS NMR. The results presented shed important new light on oxygen migration processes occurring at the a I β-phase transition of this material. A full structure solution is presented for 2-[4-(2-hydroxy-ethylamino)-6-phenylamino-[1,3,5]triazin-2-ylamino]-ethanol from powder X-ray data, an organic material investigated as part of a study of ink-jet-dyes.

Item Type:Thesis (Doctoral)
Award:Doctor of Philosophy
Thesis Date:2003
Copyright:Copyright of this thesis is held by the author
Deposited On:01 Aug 2012 11:37

Social bookmarking: del.icio.usConnoteaBibSonomyCiteULikeFacebookTwitter