³⁵ Cl Nuclear Quadrupole Resonance, NQR, spectra of mixtures of Chloromethane and Benzene, with relative molar compositions in the range 1:3 to 3:1, and at temperatures in the range 77 K to 180 K, reveals the presence of a new crystalline phase, in addition to that of pure Chloromethane. The temperature-dependence and the deuterium isotope effect of this new resonance show that the chloromethane molecule is much more labile in the new crystalline phase than in pure chloromethane. The existence of the new crystalline phase is confirmed by Differential Thermal Approach, DTA, which in addition provides evidence that the complex has a 1:1 composition and that the enthalpy of fusion is ≈ 660 cal./mole. Raman spectroscopy provides further evidence of the existence of the complex.