Addition Compounds of Phosphorus(V) Chloride and Aromatic Nitrogen Bases. Crystal Structure and 1H NMR and Raman Spectra of Pyrazine-Phosphorus(V) Chloride
The solid-state structure of a nonionic adduct of phosphorus(V) chloride and pyrazine, C4H4N2-PCI5, shows phosphorus to be six-coordinate with one octahedral position occupied by a nitrogen atom of the pyrazine ring. The monoclinic crystal is of space group C2/c having four molecules per unit cell of dimensions a = 8.359 (8) A, b = 16.202 (15) A, c = 7.568 (7) A, and p = 99.37 (7)'. The structure was refined by least squares to R = 0.097 by using 1754 independent reflections collected to 28, = 65" and corrected for absorption. The P-N distance is 2.021 (5) A. In nitromethane solution, Raman, 'H NMR, cryoscopic, and conductivity measurements are interpreted in terms of equilibria involving CIH4N2.PCIS, pyrazine, molecular PCI,, and ions originating from the ionization of PCls and C4H4N2.PClS.
The authors thank Dr. Perry P. Yaney and the University of Dayton Research Council for their assistance. In addition, acknowledgment is made to the donors of the Petroleum Research Fund, administered by the American Chemical Society, for partial support of this research. Registry No. pyz.PC15, 64537-03-7; py-PClS, 18534-27-5
American Chemical Society
Petroleum Research Fund, American Chemical Society
Meyers, B. N.; Ishley, J. N.; Fratini, Albert; and Knachel, Howard, "Addition Compounds of Phosphorus(V) Chloride and Aromatic Nitrogen Bases. Crystal Structure and 1H NMR and Raman Spectra of Pyrazine-Phosphorus(V) Chloride" (1980). Chemistry Faculty Publications. 46.