Cationic nickel(II) complexes containing chelating O,O 0 -donor maltolate or ethyl maltolate ligands in conjunction with bidentate bisphosphine ligands Ph 2 P(CH 2 ) n PPh 2 were prepared by a one-pot reaction starting from nickel(II) acetate, bisphosphine, maltol (or ethyl maltol), and trimethylamine, and isolated as their tetraphenylborate salts. An X-ray structure determination of [Ni(maltolate)(Ph 2 PCH 2 CH 2 PPh 2 )]BPh 4 shows that the maltolate ligand binds asymmetrically to the (slightly distorted) square-planar nickel(II) center. The simplicity of the synthetic method was extended to the synthesis of the known platinum(II) maltolate complex [Pt(maltolate)(PPh 3 ) 2 ]BPh 4 which was obtained in high purity.