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Two simple biphenyl-appended (2-pyridyl)alkylamine N -bidentate ligands, L e and L m , having ethylene and methylene spacers between donor groups, with bite angles L e ≈ 100° and L m ≈ 80°, dictate pseudotetrahedral and trigonal-bipyramidal geometries in six high-spin Ni(II)-halide complexes, [Ni(L e )X 2 ] and [Ni(L m ) 2 X](ClO 4 ) (where X = Cl - , Br - , I - ), respectively. The structures in the solid state, determined using X-ray crystallography, and in solution, determined using spectroscopic methods (UV-vis-NIR and paramagnetic 1 H NMR), which complement each other, are described.

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Bite-Angle-Regulated Coordination Geometries: Tetrahedral and Trigonal Bipyramidal in Ni(II) with Biphenyl-Appended (2-Pyridyl)alkylamine N,N′-Bidentate Ligands