In this paper, the synthesis, crystal structure, properties and thermoanalysis of o-vanillin glycine tripyridine Nickel(II) were reported. The complex is monoclinic system, space group is C2/c, with cell parameters a = 3.3549(6), b = 1.1396(4), c = 1.4555(5) nm, beta = 113.96(3)-degrees, V = 5.086 nm3, M(r) = 526.21, Z = 8, D(c) = 1.37 g/cm3, mu = 8.06 cm-1, F(000) = 2200. The kinetics of thermal decomposition of the complex was studied also under non-isothermal condition by TG, DTG curves. The mechanism is three-dimension diffusion, 3D (sphere symmetry). The kinetic equation is expressed as: dalpha/dt = A . e(-E/RT) . 3/2 . (1-(1-alpha)1/3]-1.