A multinuclear solid-state magnetic resonance study of silver nitrate triphenylphosphine

Variable-temperature solid-state (31)P, (15)N, and (2)H NMR spectroscopy, X-ray diffraction, and differential scanning calorimetry studies of the 1: 1 adduct of silver nitrate and triphenylphosphine (AgNO(3)center dot PPh(3)) reveal a solid-solid phase transition at 300 K. The principal components of the phosphorus and nitrogen chemical shift tensors for both phases are determined from NMR spectra of MAS and stationary samples. In addition, the indirect spin-spin coupling between phosphorus and the naturally occurring isotopes of silver ((107)Ag and (109)Ag) are resolved. Experimental 2H NMR line shapes for silver nitrate perdeuterated triphenylphosphine are those characteristic of rigid phenyl groups at temperatures above and below the phase-transition temperature. Powder and single-crystal X-ray diffraction data for AgNO(3)center dot PPh(3) obtained at 193, 295, and 313 K are reported; data obtained at 193 and 295 K are almost identical, but are significantly different from those obtained at 313 K and from an earlier single-crystal X-ray diffraction investigation performed at 298 K. All X-ray studies found that AgNO(3)center dot PPh(3) crystallizes in the monoclinic form, space group P2(1)/c.