Abstract
Crystalline 1, 3-dimethyl-2, 2, 2, 4-tetrachloro-4-trichloromethyl-1, 3, 2-diazaphosphetidine (I) has been made by rapid cooling from the liquid, which is unstable under normal conditions. I has a trigonal-bipyramidal environment for the phosphorus atom, as has been demonstrated by35Cl NQR spectroscopy, while the nitrogen atoms in the four-membered heterocyclic have an axial equatorial position. I is stable at 77 K but on temperature rise is converted to the isomeric N, N-dimethyltrichloroacetamidinium tetrachiordphosphorate (II). The I → II chlorotropic transformation is accompanied by the coexistence of the two isomeric forms in the crystal.
Literature cited
V. I. Kal'chenko, V. V. Negrebetskii, R. B. Rudyi, et al., “Chlorotropism in the C-N-P triad in N, N-dimethyltrichloro(trifluoro)acetamidinium tetrachlorophosphorates,” Zh. Obshch. Khim.,53, No. 4, 932–934 (1983).
E. A. Romanenko, V. I. Kal'chenko, and R. B. Rudyi, “Nuclear quadrupole resonance for amidinium tetrachlorophosphorates,” Teor. Éksp. Khim.,21, No. 6, 727–730 (1985).
D. E. Woessner and H. S. Gutowsky, “Nuclear pure quadrupole relaxation and its tempera- ture dependence in solids,” J. Chem. Phys.,39, No. 2, 440–456 (1963).
I. V. Izmest'ev and V. S. Grechishkin, “35Cl quadrupole spin-lattice relaxation in compounds containing chloromethyl groups,” Zh. Strukt. Khim.,11, No. 5, 927–928 (1970).
Yu. G. Shermolovich, E. A. Romanenko, T. D. Petrova, et al., “Structure and dimer-monomer conversion in trichlorophosphazopentafluorophenyl,” Izv. Sib. Otd. Akad. Nauk SSSR, Ser. Khim., No. 10, Issue 4, 70–76 (1980).
Author information
Authors and Affiliations
Additional information
Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 237–240; March–April, 1989.
Rights and permissions
About this article
Cite this article
Romanenko, E.A. Preparation and chlorotropic transformation of crystalline diazaphosphetidine. Theor Exp Chem 25, 216–218 (1989). https://doi.org/10.1007/BF01135015
Received:
Issue Date:
DOI: https://doi.org/10.1007/BF01135015