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Hydrogen Bonding Network in Interlayer Spaces of a Partially Deuterated Layered α-Sn (IV) Phosphate: A Solid-State
Vladimir I Bakhmutov1, Hong-Cai Zhou1
1Department of Chemistry, Texas A&M University, College Station, Texas, USA.
None:
Samples of a layered α-Sn (IV) phosphate were partially deuterated by soaking with D2O to yield a mixture of two isotopomers Sn (HPO4) (DPO4).c-H2O and Sn (DPO4)2.c-H2O containing cavity water c-H2O. They were characterized by the 1H, 2H, 31P, and 119Sn MAS NMR experiments including relaxation time measurements. The formation of these isotopomers is proven by the kinetic proton-deuterium cross-polarization MAS NMR experiments giving the cross-polarization rate constant TH-D of 3.2 ms. In agreement with their formulation the 2H MAS NMR spectra of Sn (HPO4) (DPO4).c-H2O and Sn (DPO4)2.c-H2O did not display the other signals besides the DPO4 resonance. The DPO4 groups observed in the temperature-independent 2H MAS NMR spectra show the DQCC value of 184 ± 6 kHz corresponding to hydrogen bonds formed with an O… O distance estimated as ~2.7 Å. Because of reduced dipolar interactions in the deuterated samples, the 1H MAS NMR spectra are well resolved providing signal assignments and the analysis. According to the solid-state NMR data collected for the partially deuterated samples of SnP, the cavity water accepts one hydrogen bond from the P-OH donor group and forms one hydrogen bond with the neighboring phosphate group, while the other water hydrogen is not involved in hydrogen bonding.
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