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A bimetallic nickel(II) complex with the ligand Hsalamp (2-[(4-methylpyridin-2-ylimino)-methyl]-phenol), having the molecular formula, Ni 2 C 26 H 22 N 4 O 10 Cl 2 , is synthesized and characterized by elemental, UV-Vis, IR and EPR studies. The IR spectrum confirms the presence of coordinated perchlorate ion and the UV-Vis. spectrum substantiates that the geometry around the metal ion is distorted square pyramidal. In the solvent methanol, the complex undergoes dissociation indicating the nature of the complex to be 1 : 2 electrolyte. The single crystal EPR studies indicate that the zero-field splitting is not large and the spectra can be observed even at room temperature, not so common for a nickel(II) ion. The spin Hamiltonian parameters calculated from single crystal rotations are: g-2⋅377, 2⋅219, 2⋅071 and D-9⋅7, 4⋅2 and-13⋅9 mT. Optical and electron paramagnetic spectral data have been used to obtain the parameters Dq, B and C.

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