In the frame of this work, we studied organometallic complexes in form of thin films oriented by corona poling. We report measurements of second and third-order nonlinear optical properties (NLO) obtained by SHG and THG techniques. For each compound studied, we determine the electronic contribution of the effective second and third-order nonlinear susceptibilities. Finally, we use X-ray diffraction to study structure of these compounds, induced by corona poling.