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In this thesis, four complexes containing N‐chloroacetyl‐salicylhydrazide （H3cashz）, N‐chloroacetyl‐5‐chlorosalicylhydrazide （H3cacshz）, N‐chloroacetyl‐5‐bromosalicylhydrazide （H3cabshz） and 4‐salicyloyl thiosemi carbazide （H3st） have been synthesized. IR, 1H NMR、13C NMR and Elemental analysis were used to characterize the compounds. X‐Ray single crystal diffraction measurements were used to characterize the crystals. And the catalytic activities of all the compounds have been studied.X‐Ray single crystal diffraction measurements were used to characterize the crystals of [Ni3 （C9 H6 N2 O3 Cl）2（C3 H7 NO）2（C5 H5 N）2], [Ni3 （C9 H5 N2 O3 Cl2 ）2（C3 H7NO）2（C5 H5 N）2] 2（C3 H7 NO）, [Ni3 （C9 H6 N2 O3 BrCl）2 （C3 H7 NO）2（C5 H5 N）2] 2（C3 H7NO） and [Ni3（C8 H6 N3 O2 S）2（C5 H5 N）2]. The crystallographic data are as follows:The complex of [Ni3（C9H6N2O3Cl）2（C3H7NO）2（C5H5N）2] is a trinuclear cluster which has been determined in the crystal system monoclinic, space group P2（1）/n, with a = 11.688（2） , b = 9.5831（17） , c = 17.226（3） ,α= 90,β= 92.015（4）,γ= 90, V= 1928.2（6） 3 , Z = 2, R1 = 0.0544, wR2 = 0.0919.The complex of [Ni3（C9H5N2O3Cl2）2（C3H7NO）2（C5H5N）2] 2（C3 H7NO） is a trinuclear cluster which has been determined in the crystal system triclinic, space group P‐1, with a = 9.2654（11） , b = 13.7345（16） , c = 20.413（2） ,α= 72.078（2）,β= 87.002（2）,γ= 84.917（2）, V = 2461.1（5） 3 , Z = 2, R1 = 0.0815,wR2 = 0.1804.The complex of [Ni3（C9H6N2O3BrCl）2（C3H7NO）2（C5H5N）2] 2（C3H7 NO） is trinuclear cluster which has been determined in the crystal system monoclinic and Triclinic. The crystal system monoclinic space group P2（1）/n, with a = 20.88（2） , b = 9.327（9） , c = 26.95（3） ,α= 90,β= 109.83（2）,γ= 90, V = 4938（9） 3, Z = 4, R1 = 0.0506, wR2 = 0.1246;The crystal system triclinic space group P‐1, with a = 9.275（9） , b = 13.777（11） , c = 20.466（19） ,α= 71.671（16）,β= 86.819（15）,γ= 84.710（19）, V = 2471（4） 3 , Z = 2, R1 = 0.0566, wR2 = 0.1157.The complex of [Ni3（C8H6N3O2S）2（C5H5N）2] is a trinuclear cluster which has been determined in the crystal system monoclinic, space group P2（1）/c, with a = 15.040（2） , b = 14.3593（19） , c = 6.2476（8） ,α= 90,β= 98.063（2）,γ= 90, V = 1335.9（3） 3 , Z = 2, R1 = 0.0484, wR2 = 0.0958.The catalytic activity for the hydrolysis of urea of all the complexes have been determined, the results show that all of four complexes have certain catalytic activity. Among the four complexes, [Ni3（C9H6N2O3Cl）2 （C3H7NO）2（C5H5N）2] has relatively strongest catalytic activity, [Ni3（C9H6 N2O3BrCl）2（C3H7NO）2（C5H5 N）2] 2（C3H7NO） has the weakest catalytic activity.
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