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Five NiII macrocyclic complexes are studied as water proton shift agents and as paraCEST agents (paraCEST = paramagnetic chemical exchange saturation transfer) for MRI applications. The five macrocycles have amide and/or alcohol pendent groups with either tetraaza‐ or triazamacrocycles including 1,1′,1′′‐(1,4,7‐triazonane‐1,4,7‐triyl)tris(propan‐2‐ol) (L1), 1,1′,1′′,1′′′‐(1,4,7,10‐tetraazacyclododecane‐1,4,7,10‐tetra)tetrakis(propan‐2‐ol)...