The synthesis, full characterization, and molecular structures of seven new coordination compounds that feature the 2‐(4′,4′‐dimethyloxazolin‐2′‐yl)thiophenolate ligand (S‐Phoz) with group 10 metals Ni, Pd, and Pt in the +II oxidation state are presented. The ML2 complexes [Pt(S‐Phoz)2] (1a), [Pd(S‐Phoz)2] (1b), and [Ni(S‐Phoz)2] (2) were prepared starting from MCl2. Compound 1a was obtained isomerically pure in a trans arrangement, whereas its Pd analogue 1b exhibits a dynamic, solvent‐dependent cis/trans equilibrium, and 2 adopts a tetrahedral arrangement. The reaction of LiS‐Phoz with [cis‐MCl2(PPh3)2] precursors resulted in full replacement of the PPh3 for M = Ni and in partial substitution for M = Pt, Pd to yield [Ni(S‐Phoz)2] (2), [Pt(κ2‐S‐Phoz)(κ1‐S‐Phoz)(PPh3)] (3a), and [Pd(κ2‐S‐Phoz)(κ1‐S‐Phoz)(PPh3)] (3b). The Pd compound 3b exhibits an interesting solvent‐dependent equilibrium with 1b and PPh3 as demonstrated by 1H and 31P NMR spectroscopy. Compounds [{PdCl(S‐Phoz)}2] (4) and [PdCl(S‐Phoz)(PPh3)] (5) were synthesized from [PdCl2(NCMe)2]. Molecular structures of compounds trans‐1a, trans‐1b, 2, 3a, 3b, 4, and 5 were determined by single‐crystal X‐ray diffraction studies. With the exception of the Ni complex 2, all compounds exhibit distorted square‐planar geometries.
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