| Salen-type bis-oxime ligand and its derivatives usually with the ability of their strong and flexible metal chelate ligands have become one of the reseach hotspots in coordination chemistry. This kind of mental complexs with the stable chemical structure in solution or in the solid condition can form single-nuclear, multi-nuclear and poly-nuclear metal complexes of Salen. Some of Salen-M complexs can be widely used in the fields of catalyses, functional materials and fundamental devices on metal liquid crystal. Therefore, Researches on the Salen-type bis-oxime ligands and its derivatives are of great significance, and the development of its performance also has the potential application value.In this thesis, the first step, we synthesized 1,2-bis(aminooxy)ethane, which was reacted with 2,6-dihydroxyacetophenone and 2-hydroxynaphthaldehyde respectively to form a kind of asymmetrical Salen-type bis-oxime ligand: 3',5-dihydroxy-[3'-methoxy-ethylenediyldioxybis(nitrilomethylidyne)]diphenol(H4L1) and one symmetrical Salen-type bis-oxime ligand: 2,2'-[Ethylenedioxybis(nitrilomethylidyne)]dinaphthol(H2L2). These ligands have been characterizated by element analysis, IR, UV and differential thermal analysis and so on. The supramolecular structures of corresponding mental complexes have also been studied and discussion.A series of new bisoxime Salen-type complexes have been synthesized by the reaction of H2L2 with Co(OAc)2·4H2O, Co(Pic)2·6H2O and Ni(OAc)2·4H2O at room temperature, respectively. The single crystals of five complexes have been grown up by methods of naturally evaporation:[{Co(L)}2{Co(Pic)2(CH3OH)2}]1,[{CoL (?-OAc)}2Co]2, [{NiL(CH3CH2OH)(?-OAc)}2Ni]3, [{NiL(CH3OH)(?-OAc)}2Ni]·2CH2Cl2·2CH3OH4 and [{NiL(CH3OH)(?-OAc)}2Ni]·1.5CH3OH5. And have been determined by X-ray crystal diffraction. The supramolecular structures, anion effect and solvent effect of these complexes have also been discussed.[{Co(L)}2{Co(Pic)2(CH3OH)2}]1:Empirical formula, C62H48Co3N10O24, Formula weight, Mr=1493.89, Monoclinic, P(2)1/c, Unit call dimensions:a= 15.0756 (5) A, b=10.7672 (3)A, c=18.6410 (7) A, p= 96.886 (2)°, Z=2, V= 3004.02(17) A3, R1=0.0593, wR2=0.1331;[{CoL(u-OAc)}2Co]2:Empirical formula, C52H42Co3N4O12, Formula weight, Mr =1091.69, Triclinic, P-1, Unit call dimensions:a= 8.9123(7) A, b= 11.9798(9) A, c =12.2170(7) A,?= 97.655(6)°, Z= 1, V= 1195.13(14) A3, R1= 0.1612, wR2= 0.1505;[{NiL(CH3CH2OH)(?-OAc)}2Ni]3:Empirical formula,C56H54N4Ni3O14, Formula weight,Mr=1183.10,Monoclinic,I12/c1,Unit call dimensions:a= 26.8222(13)A,b=9.2931(3)A,c=23.5557(12)A,?=117.932(6).,Z=4,V= 5187.5(4)A3,R1,=0.0508,wR2=0.1223?[{NiL(CH30H)(?-OAc))2Ni]·2CH2Cl2·2CH30H4:Empirical formula, C58H62N4Ni3016Cl4,Formula weight,Mr=1389.05,triclinic,P-1,Unit call dimensions:a=13.8763(8)A,b=14.7997(11)A,c=15.8806(14)A,?=84.270(6)°, Z=2,V=3037.8(4)A3,R1=0.0598,wR2:0.1507;[{NiL(CH30H)(?-OAc))2Ni]·2CH30H5:Empirical formula,C56H55N4Ni3O16, Formula weight,Mr=1202.17,Triclinic,P-1,Unit call dimensions:a=12.5014(6)A, b=14.7093(7)A,c=15.3567(9)A,?=91.713(4)°,Z=1,V=2635.8(3)A3,R1= 0.0675,wR2=0.1814?... |
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