Abstract
The new ionic intercalation compound (NH + 4) 0.22TiS 0.22− 2 has been synthesized by vacuum deintercalation of ammoniated TiS 2, characterized by thermogravimetric analysis and powder X-ray diffraction, and examined by SQUID magnetometry (indirectly), differential scanning calorimetry, incoherent inelastic neutron scattering, and nuclear magnetic resonance. Although the diffraction pattern of this compound resembles a stage-II structure in which every other van der Waals gap is occupied by NH + 4 it cannot be indexed completely on this basis. Magnetic and calorimetric measurements show that one electron is transferred to the host TiS 2 conduction band per NH + 4 cation and that the deintercalation enthalpy of NH + 4 is 22 kcal/mol NH + 4, respectively. Neutron scattering has provided evidence for an NH + 4 torsional fundamental mode at 215 cm −1. The proton NMR linewidth and spin-lattice relaxation time are independent of temperature between 100 and 540 K, and the linewidth of 2.6 ± 0.3 G is in good agreement with that calculated for isotropic reorientation of the NH + 4 cations.
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