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The dinickel(II) dihydride complex ( 1 K  ) of a pyrazolate‐based compartmental ligand with β‐diketiminato (nacnac) chelate arms (L − ), providing two pincer‐type {N 3 } binding pockets, has been reported to readily eliminate H 2  and to serve as a masked dinickel(I) species. Discrete dinickel(I) complexes ( 2 Na  ,  2 K  ) of L −  are now synthesized via a direct reduction route. They feature two adjacent T‐shaped metalloradicals that are antiferromagnetically coupled, giving an  S =0 ground state. The two singly occupied local    d    x  2   -   y  2type magnetic orbitals are oriented into the bimetallic cleft, enabling metal–metal cooperative 2 e −  substrate reductions as shown by the rapid reaction with H 2  or O 2 . X‐ray crystallography reveals distinctly different positions of the K +  in  1 K   and  2 K  , suggesting a stabilizing interaction of K +  with the dihydride unit in  1 K  . H 2  release from  1 K   is triggered by peripheral γ‐C protonation at the nacnac subunits, which DFT calculations show lowers the barrier for reductive H 2  elimination from the bimetallic cleft.

Ligand Protonation Triggers H 2 Release from a Dinickel Dihydride Complex to Give a Doubly “T”‐Shaped Dinickel(I) Metallodiradical