A computer controlled 4π‐Zeeman split pulse fourier transform NQR spectrometer has been constructed. The NQR spectra for more than 200 different magnitutes and orientations of the magnetic field in the sphere can be obtained and stored under software control. This allows an almost fully automatic determination of the zero splitting cones by refining grids of field orientations in the space. — The crystal structure of p‐chloroanilinium trichloroacetate (4‐ClC6H4NH⊕3) (Cl3CCOO⊖), has been determined (C52h ‐ P21/c, z = 4, a = 942.3 pm, b = 722.8 pm, c = 1748.6 pm, β = 100.54°). — The direction cosines of the principal axes and the asymmetry parameters η of the electric field gradient tensors have been obtained together with the nuclear quadrupole coupling constants e2Qφzzh−1 of the chlorine atoms of the CCl3 group (η(1) = 0.0255, e2Qφzzh−1 (35Cl(1)) = 76.790 MHz, η(2) = 0.0355, e2Qφzzh−1 (35Cl(2)) = 76.410 MHz, η(3) = 0.0132, e2Qφzzh−1 (35Cl(3)) = 75.910 MHz and of the chlorine atom bound to the ring (η(4) = 0.0996, e2Qφzzh−1 (35Cl(3)) = 69.244 MHz) at T = 295 K. — The frequencies v(35Cl), linewidths Δv(35Cl) and the spin lattice relaxation times T1(35Cl) have been investigated as function of temperature for v1…v4 and the activation energy for the bleaching out process has been calculated from the Δv = f(T) data (Ea = 65 kJmol−1) and T1 = f(T) data (Ea = 72 kJmol−1). The results are discussed in context with the crystal structure.
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