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The ability of bridging thiophenolate groups (RS − ) to transmit magnetic exchange interactions between paramagnetic Ni II  ions is examined. Specific attention is paid to complexes with large NiSRNi angles. For this purpose, dinuclear [Ni 2 L 1 (μ‐OAc)⋅I 2 ][I 5 ] ( 2 ) and trinuclear [Ni 3 L 2 (OAc) 2 ][BPh 4 ] 2  ( 3 ), where H 2 L 1  and H 2 L 2  represent 24‐membered macrocyclic amino‐thiophenol ligands, are prepared and fully characterized by IR‐ and UV/Vis spectroscopy, X‐ray crystallography, static magnetization  M  measurements and high‐field electron spin resonance (HF‐ESR). The dinuclear complex  2  has a central N 3 Ni 2 (μ‐S) 2 (μ‐OAc)Ni 2 N 3  core with a mean NiSNi angle of 92°. The macrocycle L 2  supports a trinuclear complex  3 , with distorted octahedral N 2 O 2 S 2  and N 2 O 3 S coordination environments for one central and two terminal Ni II  ions, respectively. The NiSNi angles are at 132.8° and 133.5°. We find that the variation of the bond angles has a very strong impact on the magnetic properties of the Ni complexes. In the case of the Ni 2 ‐complex, temperature  T  and magnetic field  B  dependencies of  M  reveal a ferromagnetic coupling  J =−29 cm −1  between two Ni II  ions (H= J S 1 S 2 ). HF‐ESR measurements yield a negative axial magnetic anisotropy ( D <0) which implies a bistable (easy axis) magnetic ground state. In contrast, for the Ni 3 ‐complex we find an appreciable antiferromagnetic coupling  J ′=97 cm −1  between the Ni II  ions and a positive axial magnetic anisotropy ( D >0) which implies an easy plane situation.

Interplay of Magnetic Exchange Interactions and NiSNi Bond Angles in Polynuclear Nickel(II) Complexes