The reaction of Ni(OH)2 and methanetrisulfonic acid trihydrate CH(SO3H)3·3H2O (H3MTA·3H2O) in N-methyl-pyrrolidone (NMP) leads to the trinuclear complex {Ni3[MTA]2(NMP)8} (triclinic, P1̅, Z=1, a=946.25(3), b=1073.24(3), c=1518.27(4) pm, α=72.193(2), β=87.398(2), γ=89.389(2)°, V=1466.49(7)×106 pm3). The structural features of the methanetrisulfonate anions are tripodal as well as chelating coordination of the Ni2+ ions. The thermal analysis has shown that the compound is first losing NMP molecules and that the solvent-free methanetrisulfonate finally decomposes yielding Ni3S2.