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Hydrothermal reaction of olsalazine sodium, phenanthroline and Zn(ClO4)2·6H2O in the presence of water and ethanol affords a two‐dimensional coordination polymer [Zn4(OSA)3(Phen)2(H2O)2]n(1) (OSA = olsalazine) which is characterized by single X‐ray determination, IR and UV spectrum. The local coordination around all zinc ions can be best described as a slightly distorted triangle bipyramid. Complex 1consists of a tetrameric subunit, which is made up of four Zn atoms bridged by four O atoms. Two types of osalazine ligands can be found in the complex according to their different coordination modes of carboxyl groups. Crystal data for 1: $\rm P{\bar 1}$, a= 10.087(7), b= 12.830(9), c= 14.545(11) Å, α =114.598(10)°, β= 92.552(10)°, γ = 108.515(10)°, V= 1588(2) Å3, Z= 2, R1= 0.0818, wR2= 0.1855. In comparison with the free ligand, the UV spectrum of 1in solution (H2O: EtOH = 1:1) shows a small Einstein shift probably due to the formation of coordination polymer and supramoleculer hydrogen‐bonding interactions.

The hydrothermal reaction of Cd(ClO4)2·6H2O and Gatifloxacin(Gati) affords a binuclear complex of Gatifloxacin, [Cd(Gati)(py)3]2·(ClO4)4(1), which is characterized by X‐ray crystallographic analysis, IR and fluorescent spectroscopy. Crystal data for 1, C34H36CdCl2FN6O12: monoclinic, P21/c, a= 18.3642(5), b= 12.8156(4), c= 16.7210(5) Å, β = 97.931(1)°, V= 3897.6(2) Å3, Z = 4. The local surrounding of the CdIIion is a slightly distorted octahedron. Solid‐state fluorescence measurements of 1at room temperature show an emission peak at 439 nm.