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Synthesis, Characterization and Catalytic Activity for Urea Hydrolysis of Multinuclear Nickel Complexes

Author: ShenYueSong
Tutor: JinLongFei
School: Central South University for Nationalities
Course: Organic Chemistry
Keywords: derivatives of salicylhydrazide synthesis characterization catalyticactivity
CLC: O643.36
Type: Master's thesis
Year: 2011
Downloads: 28
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Abstract


Salicylhydrazides have good biological activity. In order to further study the synthesis and properties of derivatives, model compounds of urease are chosen as the object of investigation. We synthesize salicylhydrazides by modifying on salicyhydrazide ligand and then react with the Ni（Ac）2·4H2O to prepare the nickel complexes. The mainly work are as following:Three salicylhydrazides have been synthesized, N,N’-bissalicyloyl- aceto- dihydrazide、N-N-bis（5-chlorosalicyloyl）-aceto-dihydrazide and ethyl 2-oxo-2-（5-bromosalicyhydrazidyl） acetate. Elemental analysis, IR, 1H-NMR, 13C-NMR were used to characterize all the compounds. X-ray single crystal diffraction measurements were used to characterize the crystals obtained from relative nickel complexes.The complex [Ni6(C16H8N4O6)2（C5H5N）6（C3H7NO）（H2O）]·3H2O is a six nuclear cluster which has been determined in the crystal system monoclinic, space group C2/c, with a=49.029（3） （?）,b=13.1355（7） （?）,c=24.2826（13） （?）,β=107.521（2）°,V=14912.9（14）（?）3,Z=4,Dcalc=0.733g/cm-3,R1=0.0976,wR2=0.2394,have 13823 diffract points with I > 2σ（I） , two center nickels are bonded with two carbonyl oxygen atoms from H6bsadhz6- and two hydrazine nitrogen atoms、one nitrogen atom from DMF and one oxygen from water. All these atoms form a six-coordinate octahedral geometry. The other four nickel ions are bonded by six nitrogen atom from pyridine, two nitrogen atom from hydrazine and two hydroxybenzene oxygen atoms to form a four-coordinate square plane.The complex [Ni6(C16H6N4O6Cl2)2（C5H5N）6（H2O）2]·2H2O is a six nuclear cluster which has been determined in the crystal system monoclinic, space group C2/c, with a = 30.531（5） （?）, b = 13.202（2） （?）, c = 22.777（4）（?）,β= 127.593（3）, V = 7274（2）（?）3, Z = 4,Dc = 1.588 g/cm3, F（000） = 3476 ,μ（Mo-ka） = 1.738 mm-1, R1 = 0.1045, wR2 = 0.2437, have 6574 diffract points with I > 2σ（I）. The two center nickels atom bonded with two carbonyl oxygen atoms from H6bcsadhz6- and two hydrazine nitrogen atoms, two oxygen from H6bcsadhz6-, all these atoms form an idea six-coordinate octahedral geometry. The other four nickel ions are bonded by six nitrogen atom from pyridine and two nitrogen atom from hydrazine and two hydroxybenzene oxygen atoms and two water form a four-coordinate square plane.The complex [Ni3(C11H8N2O5Br)2（C5H5N）4] is a three nuclear cluster which has been determined in the crystal system monoclinic, space group P2（1）/n, with a = 9.823（7） （?）, b = 9.803（7） （?）, c = 22.992（17）（?）,β=100.488（15）, V = 2177（3）（?）3, Z = 2, Dc = 1.752 g/cm3, F（000） = 1156 ,μ（Mo-ka） = 3.187 mm-1, R1 =0.0832, wR2 = 0.1643 have 4032 diffract points with I > 2σ（I）. The center nickel atom is bonded by two nitrogen atoms from pyridine and two carbonyl oxygen atoms from H3eobshza3- and two hydrazine nitrogen atoms, all these atoms form an idea six-coordinate octahedral geometry. The other two nickel ions are bonded by one nitrogen atom from pyridine and one nitrogen atom from hydrazine and two hydrazine oxygen atoms, all these atoms to form a four-coordinate square plane.The catalytic activity of the nickel complexes has been studied. For the hydrolysis of urea, the results of modulation of urease show that the six nuclear nickel clusters have better activity than the three nuclear nickel clusters.

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CLC: > Mathematical sciences and chemical > Chemistry > Physical Chemistry ( theoretical chemistry ),chemical physics > Chemical kinetics,catalysis > Catalytic > Catalyst
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