| Two intermediates were obtained by the reaction of 4-aminophenone with methoxylamine hydrochloride and ethoxylamine hydrochloride.At the same time,the obtained and purified intermediates react with 5-nitro salicylaldehyde and 3,5-dichloro salicylaldehyde,then three kinds of organic Schiff base ligands are obtained,they are used for a series of complexation reactions with salt of transition metal,and had got some complexes.By single crystal X-ray diffraction,the following crystal data are obtained.Respectively,HL1?HL3?[Cu(L1)2]?[Co(L1)2]?[Co2(L2)4]?[Zn(L2)2]?[Zn(L3)2]and[Fe2(L3)4·H2O].The ligands and their complexes were characterized by IR and fluorescence spectra.What is more,the hydrogen bonds in the complexes were also studied.Crystal 1:Empirical formula,C16H14Cl2N2O2,Formula weight,337.19,monoclinic,P 21/c,a=7.9157(6)A,b=13.4533(8)A,c=14.8459(10)A,?=90.00°,?=103.651(2)°,?=90.00°,Z=4,V=1536.31(18)A3,R1=0.0389,wR2=0.1124;Crystal 2:Empirical formula,C16H15N3O4,Formula weight,313.31,monoclinic,P 21/c,a=6.4730(5)A,b=8.1564(6)A,c=27.511(2)A,?=90.00°,?=90.113(2)°,?=90.00°,Z=4,V=1452.48(19)A3,R1=0.0448,wR2=0.1043;Complex 1:Empirical formula,C32H28Cl4CuN4O5,Formula weight,753.92,monoclinic,P 21/n,a=14.584(4)A,b=14.210(4)A,c=16.643(5)A,?=90.00°,?=110.699(5)°,?=90.00°,Z=2,V=3226.4(16)A3,R1=0.0848,wR2=0.2443;Complex 2:Empirical formula,C32H26Cl4CoN4O4,Formula weight,731.30,monoclinic,C c,a=17.2101(17)A,b=16.3985(19)A,c=22.906(2)A,?=90.00°,?=102.041(3)°,?=90.00°,Z=8,V=6322.3(11)A3,R1=0.0513,wR2=0.0841;Complex 3:Empirical formula,C69H62Cl10Co2N8O8,Formula weight,1603.63,triclinic,P-1,a=10.790(5)A,b=14.587(7)A,c=22.966(11)A,?=82.780(9)°,?=82.489(9)°,?=79.006(9)°,Z=2,V=3499(3)A3,R1=0.0793,wR2=0.2357;Complex 4:Empirical formula,C34H30Cl4N4O4Zn,Formula weight,765.81,triclinic,P-1,a=10.5785(8)A,b=14.6788(11)A,c=23.1472(17)A,?=83.538(1)°,?=82.354(1)°,?=79.854(1)°,Z=4,V=3492.0(5)A3,R1=0.0378,wR2=0.1078;Complex 5:Empirical formula,C32H28N6O8Zn,Formula weight,689.99,monoclinic,C 2/c,a=26.940(5)A,b=5.6721(12)A,c=23.647(5)A,?=90.00°,?=123.631(4)°,?=90.00°,Z=4,V=3008.6(11)A3,R1=0.0795,wR2=0.1835;Complex 6:Empirical formula,C64H56Fe2N12O17,Formula weight,1376.91,triclinic,P-1,a=12.5150(8)A,b=15.3703(10)A,c=16.4718(11)A,?=92.070(2)°,?=91.283(2)°,?=100.655(2)°,Z=2,V=3110.5(4)A3,R1=0.0622,wR2=0.1538;... |
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