31P multiple-quantum solid-state NMR spectroscopy is
introduced as a new approach for elucidating
internuclear distances between phosphorus nuclei in phosphates.
The typical shorter distance between chemically
bound groups allows the determination of the chemical network. The
method is superior to 31P exchange
experiments,
which, in principle, provide similar information. Separation of
two crystalline Mg2P2O7 phases is
observed by both
methods, but the double-quantum experiment gives further information of
couplings between sites with equal isotropic
chemical shifts. In Ca2P6Ol7,
which contains Q2 and Q3 groups with large
chemical shift anisotropies, the connectivities
can be deduced from the double-quantum experiment due to different
cross-peak intensities. Our results are in good
agreement with X-ray diffraction measurements and suggest applications
to other, more complicated phosphates.
It is demonstrated on a polycrystalline powder sample of
Cd3(PO4)2, given a known
single-crystal X-ray
structure, that two-dimensional 31P double-quantum
single-quantum MAS correlation experiments allow unique
assignment of multiple 31P resonances to specific P sites
in the structure of such inorganic orthophosphates.
The
eigenvalues of the 31P and 113Cd shielding
tensors of Cd3(PO4)2 are reported,
the determination of which requires
usage of a 2D MAS spinning sideband separation experiment.
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