The molecular structure of 4 with anisotropic displacement parameters depicted at the 50 % probability level. Hydrogen atoms are not shown for clarity. Selected bond lengths (Å) and bond angles (°): Ni1−N1 1.8789(9), Ni1−N2 1.8923(9), Ni1−N3 1.9063(10), Ni1−S1 2.2330(3); N1−Ni1−N2 94.39(4), N1−Ni1−N3 83.81(4), N2−Ni1−N3 163.60(4), N1−Ni1−S1 164.36(3), N2−Ni1−S1 93.04(3), N3−Ni1−S1 92.83(3), C1−S1−Ni1 106.76(4). CCDC: 2271418.

The molecular structure of 4 with anisotropic displacement parameters depicted at the 50 % probability level. Hydrogen atoms are not shown for clarity. Selected bond lengths (Å) and bond angles (°): Ni1−N1 1.8789(9), Ni1−N2 1.8923(9), Ni1−N3 1.9063(10), Ni1−S1 2.2330(3); N1−Ni1−N2 94.39(4), N1−Ni1−N3 83.81(4), N2−Ni1−N3 163.60(4), N1−Ni1−S1 164.36(3), N2−Ni1−S1 93.04(3), N3−Ni1−S1 92.83(3), C1−S1−Ni1 106.76(4). CCDC: 2271418.

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The reaction of a nickel(II) chloride complex containing a tridentate β‐diketiminato ligand with a picolyl group [2,6‐iPr2‐C6H3NC(Me)CHC(Me)NH(CH2py)]Ni(II)Cl (1)] with KSi(SiMe3)3 conveniently afforded a nickel(I) radical with a T‐shaped geometry (2). The compound‘s metalloradical nature was confirmed through electron paramagnetic resonance (EPR)...