Abstract (PDF) Graphical Abstract: This paper reports on the synthesis and structure re-refinement of bis(lidocaine) diaquatetrathiocyanatonickelate(II). The compound with the formula (LidH)2[Ni(NCS)4(H2O)2], where Lid is (2-(diethylamino)-N-(2,6-dimethylphenyl)acetamide, crystallizes in the monoclinic space group P21/c with a= 18.3509(5), b= 7.6532(2), c= 14.9585(4) Å, β= 109.964 (2)°, V= 1974.57 (9) Å3, and Z= 2. Coordination of the Ni2+ ion with thiocyanate ions and water molecules generates slightly distorted octahedral anion [Ni(NCS)4(H2O)2]2– with N-bonded thiocyanate groups, while two protonated cations LidH+ remain in an outer coordination field.