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The novel three-dimensional chiral framework of the four-coordinate zinc complexes, [Zn 4 (biim) 3 (ina) 2 ] ( 1a and 1b ) (H 2 biim = 2,2′-biimidazole, ina = isoniconate), has been prepared via hydrothermal reaction. X-ray single crystal diffraction analysis shows the biim 2− in title complexes acts as a tetradentate ligand and links four different Zn 2+ ions. Spontaneous chiral resolution occurs in solvo-thermal reaction, which was confirmed by solid-state circular dichroism spectra. Photoluminescent spectra of compound 1 exhibit an intense blue emission at 440 nm.