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Two novel dithiophosphonate ligands, HS2P(p‐C6H4OMe)(OCH2CH2CH(CH3)2) (1) and HS2P(p‐C6H4OMe)(OCH(CH3)2) (2), were synthesized and characterized by multinuclear (1H, 31P, and 13C) NMR, infrared spectroscopy as well as elemental analysis. The reactions of 1 and 2 with NiCl2·6H2O and Cd(NO3)2·4H2O in methanol led to novel complexes 3 and 4. The single crystal X‐ray structures of 3 and 4 showed tetracoordinated structure with square planar geometry for the nickel complex, while it showed pentacoordinated structure with distorted square‐pyramid environment for the cadmium complex.

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