水楊酰肼衍生物及其金屬冠醚配合物的合成、表征與酯化反應(yīng).pdf

1、華中師范大學(xué)碩士學(xué)位論文水楊酰肼衍生物及其金屬冠醚配合物的合成、表征與酯化反應(yīng)姓名：余慧申請學(xué)位級別：碩士專業(yè)：應(yīng)用化學(xué)指導(dǎo)教師：金龍飛20090501⑨碩士學(xué)位論文MASTER’STHESISAbstractMetallacrowncompoundisanewtypeofmaerocycliccompoundstructurallysimilartometalclusterSalicylhydrazidederivativeisone

2、ofthemostimportantligandsformetallacrownssynthesisInthethesis，threenewtrianionicheptadentateligands，(z)一3一(salicylhydrazinocarbonyl)propenoicacid((z)一Ihshcpa)，(z)一3一(5’一chlorosalicylhydrazinocarbonyl)propenoieacid((z)H4c

3、shcpa)and(z)一3一(5’bromosalicylhydrazinocarbonyl)propenoicacid(固一H4bshcpa)，weresynthesizedandreactedwithFeCl36H20，respectivelyThree18一metallacrown6complexeshavebeenobtainedElementalanalysis，IR1HNMRand13CNMRwereusedtochara

4、cterizethreecompoundsrespectivelyandtheXRaywereusedtoconfLrmthree18metallacrown6crystalsNovelcomplex[Fe兒16(C12HgN20s)6(H20)2(CHsOH)4]。6CH30HcrystallizesinthemonoclinicsystemandspacegroupC2／c，wherea=13576(10)A，b=15536(12)

5、A薩16419(12)A，V=2943(4)A3，Z=1，RI=00332，wR2=O0811，GOF=I105Novelcomplex[Fe16(C12H8N20sCI)6(I120)4(CH30H)2]‘8H20。4CH30HCrystallizesinthetriclinicsystemandspacegroupP1，wherea=13576(10)A，6=15536(12)Ac=16419(12)AV=2943(4)Ⅳ，Z_l，

6、Rl=O0332，wR2=O0811，GOF=I105Novelcomplex[Fe川6(C12H8N20sBr)6(H20)2(CH30H)4】。8H20。8CH30HCrystallizesinthetficlinicsystemandspacegroupP1，wherea=13551(2)A，b=15571(2)Ac=16423(3)A，V=29417(8)A’，Zr=1，RI=00534，wR2=O1584，GOF=I121Si

7、nglecrystalXraystructureanalysisofthreecomplexesshowedthatallneutralFe(III)complexescontaineda18memberedmetallacrownringconsistingofsixFe(III)andsixtrianionicligandsAll18一memberedmetallaerownringisformedbytheSUCCESSionof

8、sixstructuralmoietiesofthetype[Fe(III)NqDuetothemeridionalcoordinati—onoftheligandstotheFe3ionstheligandsenforcethestereochemistryoftheFe3ionsasapropellerconfiguration、析t11alternatingA／△formsIntheselfassemblyprocessallli

9、gandswereesterifiedInthehydrochloricacidsolutionthesemetallaerownsCanbetreatedwithSnCl2‘2H20toobtainpurifiedesters，including(刁一methyl3一(salicylhydrazinocarbonyl)propenoate(∞H3mshcp))，(z)methyl3一(5’一chlorosalicylhydrazino

10、carbonyl)propenoate((z)一Hsmcshcp))and(z)methyl3一(5’一bromosalicylhydrazinocarbonyl)propenoate“刁一H3mbshcp))；Inadditionwehavealsoobtainedreducedesterifiedligandsrespectively、析manotherreductantZnpowder，includingmethyl3(salic