A new microporous organic-inorganic hybrid organosilica LHMM-2 containing a bis(propyliminomethyl)benzene moiety inside the framework has been synthesized hydrothermally without using any template or structure-directing agent. Powder XRD and TEM image analyses suggest a new disordered microporous structure with pores of dimension ca. 0.54 nm, and (13)C and (29)Si MAS NMR and spectroscopic results indicate the presence of bridging organic bis(propyliminomethyl)benzene moiety in this framework. TPD-NH(3) results suggested that nearly 5 times as much bis(propyliminomethyl)benzene moiety is located inside the micropore walls (matrix) than in the surface of the pores. LHMM-2 shows very high adsorption capacity for metal cations like Fe(3+), Cu(2+) and Zn(2+).