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Abstract: Solid-state NMR methods based on dipolar and J-derived experiments such as CP, MAS-J-HMQC and MAS-J-INEPT MAS have been developed in the frame of the {31P,29Si} spin pair. The potential of these techniques has been demonstrated using model compounds including crystalline silicophosphate phases (Si5O(PO4)6 and various SiP2O7 polymorphs). Spatial interactions as well as through-bond connectivities were established. Evaluation of isotropic 2 J P–O–Si coupling constants has been established by careful analysis of the HMQC and INEPT build-up curves under fast MAS. The efficiency of the 31P→ 29Si CP MAS experiment for the detailed characterization of Si–O–P mesoporous materials (at low temperature) was demonstrated. The incorporation of P atoms in the silica network has been proved unambiguously. Such materials could be appropriate for biocompatibility purposes. [Copyright &y& Elsevier]