Pb2(TNR)(NO3)2(H2O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb2(TNR)(NO3)2(H2O)was determined by single crystal diffraction analysis. The crystal is triclinic, space group with crystal parameters a=0.7279(2)nm,b=1.0698(2)nm,c=1.0738(2)nm;α=86.82(1)°,β=89.52(2)°,γ=83.50(2)°;V=0.8295(3)nm3,Z=2,Dc=3.201g·cm-3, F(000)=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.