Solid state NMR spectroscopy - Framework Structure

Framework Structure

7.2.2 Solid state NMR spectroscopy

31_P{1_H}_{MAS NMR experiments were carried out on a BRUKER Avance II spectro-}

meter equipped with a commercial 2.5 mm MAS NMR double resonance probe at a mag- netic field strength of 4.7 T. The chemical shift values refer to a deshielding scale and 85 % H3PO4 used as an external reference. The C-REDOR experiment and the determi-

nation of the principle components were carried out as described in the literature.[54,55] Up to 1.2 ms on the unified dephasing scale, no dephasing was observed in the C-REDOR curves (see Figure 6). Hence 1H-31P spin pairs at a distance smaller than approximately 1 pm can be ruled out at the noise level of the experiment. Together with half the maximum P–P distance in the unit cell, this proves the absence of H atoms in Sr3P6O6N8.

Figure 6. 31_P{1_{H}-CREDOR curve of the}31_{P resonance of Sr3P6O6N8; the experimental conditions are the} same as those used in reference [54].

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In document Sedlmaier, Stefan (2011): Synthesis, identification and characterization of novel, condensed oxonitridophosphates and phosphorus oxonitrides. Dissertation, LMU München: Fakultät für Chemie und Pharmazie (Page 111-116)