The formation of unique nanometer-sized organic supramolecular assemblies was observed in the lamellar space of metal phosphate host lattices. Two new chiral and achiral organic-inorganic hybrid materials, zinc phosphate, (H 3 tren) 2 [Zn 3 (PO 4 ) 4 ] . 2NDA(ZnP-NDA) and zinc-cobalt phosphate, (H 3 tren) 2 [Zn 1.6 Co 1.4 (PO 4 ) 4 ] . 2NDA (ZnCoP-NDA) have been synthesized under hydrothermal conditions. The crystalline host framework was built with corner-sharing MO 4 (M=Zn or Zn/Co) and PO 4 tetrahedra. In between these framework layers, aromatic dicarboxylic acid, 2,6-Naphthalene dicarboxylic acids (NDA) are held together by means of strong hydrogen bonding and π-π stacking interactions resulting in infinite supramolecular zigzag chains. After incorporating the cobalt into inorganic host lattice, astonishingly, the chiral structure tuns achiral. The crystal structures were elucidated by single crystal X-ray diffraction and characterized by powder XRD, elemental analysis, thermogravimetry and photoluminescence measurements.