Two new organic-inorganic hybrid materials, based on 1,3-CycloHexaneBis-(Methyl Amine), abbreviated CHBMA, namely (H(2)CHBMA)ZnCl4 center dot 2H(2)O (CP1) and (H(2)CHBMA)CdI4 center dot 2H(2)O (CP2), have been synthesized under mild conditions in acidic media and characterized by single-crystal X-ray diffraction, spectroscopic techniques (C-13 NMR, FTIR, RAMAN) and thermal analysis. The crystal structures of the two compounds were solved by single-crystal X-ray diffraction methods. Both compounds show a 3-dimensional supramolecular structure directed by various interactions between tetrahalidometallate anions (ZnCl42-, CdI42-), water molecule and organic cations (H(2)CHBMA)(2+). For both compounds, the cyclohexane ring of the template cation is in a chair conformation with the methylammonium substituent in the equatorial positions and the two terminal ammonium groups in a cis conformation but with two different orientations (upward for CP1 and downward for CP2) which influences the supramolecular architecture of the two structures. Hirshfeld surface analysis and the associated two-dimensional finger print plots were used to explore and quantify the intermolecular interactions in the crystals.