[Pb-2(TNR) (NO3)(2)(H2O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb-2(TNR) (NO3) (2)(H2O) was determined by single crystal diffraction analysis. The crystal is trielinic, space group P (1) over bar with crystal parameters a = 0. 7279 (2) nm, b = 1. 0698 (2) nm, c = 1. 0738(2) nm; alpha = 86. 82(1)degrees, beta = 89.52(2)degrees, gamma = 83.50 (2) degrees; V = 0. 8295 (3) nm(3), Z = 2, D-c = 3. 201g . cm (-3), F(OOO) = 716. The final R value is 0.0358. In the crystal structure, one lead ion was represented by nine coordination geometry; the other was showed as ten coordination geometry.