The First Observation of Heteronuclear Two-BondJ-Coupling in the Solid State: Crystal Structure and Solid-State NMR Spectroscopy of Rb4(NbO)2(Si8O21)

High-temperature, high-pressure hydrothermal synthesis of the title compound and its (93)Nb and (29)Si MAS NMR spectra are reported. The (29)Si MAS NMR spectrum shows four signals corresponding to the four distinct Si sites in the structure. Three signals show multiplet patterns which arise from (93)Nb(spin-(9)/(2))-(29)Si J-coupling. This is the first example of two-bond J-coupling between a quadrupolar nucleus and a spin-(1)/(2) nucleus in the solid state. A combination of (93)Nb and (29)Si solid-state NMR and X-ray diffraction data has provided a correlation between NMR interaction parameters and local structure. This work opens a new opportunity to examine the relationship between (2)J-coupling and structural parameters in the solid state.