Abstract: | Vibrational Spectra of Trimethylphosphonium Cations (CH3)3PX+ (X = H, D) and Crystal Structures of (CH3)3PD+SbCl6? and (CH3)3PCl+SbCl6? The trimethylphosphonium salts (CH3)3PX+SbCl6? (X = H, D) and (CH3)3PH+MF6? (M = As, Sb) are prepared and characterized by vibrational and NMR spectroscopy (1H, 31P, 13C). In addition the crystal structures of (CH3)3PD+SbCl6? and (CH3)3PCl+SbCl6? are reported. (CH3)3PD+SbCl6? crystallizes in the orthorhombic space group Pnma with a = 1555(1) pm, b = 753.1(8) pm, c = 1166(1) pm Z = 4. (CH3)3PCl+SbCl6? crystallizes triclinic in the space group P1 with a = 704.6(4) pm, b = 729.5(3) pm, c = 1391.1(7) pm, α = 89.57(4)°, b? = 88.04(4)°, γ = 74.98(4)° and Z = 2. |