SYNTHESISCRYSTAL STRUCTURES AND BIOLOGICAL ACTIVITY OF TRINUCLEAR NICKEL(II) AND COPPER(II) COMPLEXES DERIVED FROM NN′ BIS(4-B.docx

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1、ISSN0022-4766,Journa1ofStructura1Chemistry,2023,Vo1.63,No.4,pp.647-657.P1eiadesPub1ishing,1td.,2023.TextTheAuthor(s)z2023,pub1ishedinZhurna1StrukturnoiKhimii,2023,Vo1.63,No.4,pp.521-523.SYNTHESIS,CRYSTA1STRUCTURESANDBIO1OGICA1activityofTrinuc1earnicke1(jandcopper()COMP1EXESDERIVEDFROMN,N-BIS(4-BROMo

2、SA11CY11DENE)13PENTANED1AMINEY.-H.Xiao1*zH.-Y.Wu1*zC.Sun1zandJ.-1.HouThese1f-assemb1yreactionofthebis-SchiffbaseNzN,-bis(4-Bromosa1icy1idene)-1,3-pntanediamine(H21)withnicke1ch1orideandsodiumazideinmethano1affordedanewpheno1ateandend-onazidebridgedtrinuc1earnicke1comp1exNi312(1,1-N3)2(CH3OH)22CH3OH(

3、1).ThereactionofH21withcopperacetateproducedanewpheno1ateandacetatebridgedtrinuc1earcoppercomp1exCu312(CH3COO)2(2).Thecomp1exeswerecharacterizedbye1ementa1ana1ysis,IRandUV-Visspectroscopy.Thecrysta1structuresofthecomp1exeshavebeendeterminedbyX-raycrysta11ography.Incomp1ex1,theNiatomsareinoctahedra1c

4、oordination,whi1eincomp1ex2,theCuatomsareinsquarepyramida1andoctahedra1coordination.TheSchiffbase1igandcoordinatestothemeta1atomsthroughthetwopheno1ateOandtwoimineNatoms.Theantimicrobia1activitiesofthecomp1exeswereassayedandeva1uated.DOI:10.1134S0022476622040175Keywords:nicke1comp1ex,coppercomp1ex,S

5、chiffbase,crysta1structures,antimicrobia1activity.INTRODUCTIONThese1f-assemb1yoforganic1igandswithmeta1atomstoformmu1tinuc1earcomp1exeshaveattractedmuchattentioninrecentyears.Schiffbasesandtheirmeta1comp1exesexhibitbio1ogica1activitysuchasantivira1,antibiotics,antibacteria1andantitumouragentsbecause

6、oftheirspecificmo1ecu1arstructures1-6.AmongtheSchiffbases,thosederivedfromthebi-condensationoforganicamineswithcarbony1compounds,areagroupofc1assica1N2O2donor1igands7-9.TheseSchiffbase1igandsreactreadi1ywithnicke1andcoppersa1tstooccupytheirbasa1orequatoria1coordinationsiteswhereassevera1anionicorneu

7、tra11igandsbindtothemeta1atomsattheapica1oraxia1positionstoyie1ddifferenttypesofcomp1exeswithvariousstructures.Amongtheco-1igands,azideandacetatehavereceivedgreatattentionbecausetheycancoordinatetothemeta1atomsthroughversati1emodes,suchasend-onandend-to-endforazide,andmonodentate,che1ating,1Co11egeo

8、fChemistryandChemica1Engineering,QiqiharUniversity,QiqihacPeop1e,sRepub1icofChina;*xiaoyinghui126,*wuhongyuan163.Origina1artic1esubmittedNovember28,2023;revisedDecember16,2023;acceptedDecember29,2023.*Supp1ementarymateria1sareavai1ab1eforthisartic1eatdoi10.1134S0022476622040175andareaccessib1eforaut

9、horizedusers.0022-4766/22/6304-06472023byP1eiadesPub1ishing,1td.647bidentatebridging,monoatomicbridging,che1atingbridging,etcforacetate(Scheme1)10-16.TocombineSchiffbasesandazideoracetatetogetherinthemeta1comp1exes,anumberofnicke1andcoppercomp1exeshavebeensynthesized.Mostnicke1andcoppercomp1exeshave

10、interestingstructures,bio1ogica1,magnetic,andcata1yticproperties17-22.However;itissti11agreatcha11engetoprepareazideoracetatebridgedmu1ti-nuc1earcomp1exeswithaimingstructures.Herein,wereportthesynthesisandcrysta1structuresoftwonewnicke1(11)andcopper(11)ComPIeXeS,Ni312(U1rN3)2(CH3OH)22CH3OH(1)andCuj1

11、z(CH3COO)2(2),where1isthedianionicformofN,N-bis(4-bromOSaIiCy1idene卜1,3-Pemanediamine(H21;Scheme2).MocMMknuiitfCc1amgBidcnUNcbdgngMonaMomkbridgingS*bencI.hc1stmodsoazdeBndctat1iamh.,.rScheme2,Thebis-SchiffbaseH21.EXPERIMENTA1Materia1sandphysica1measurements.A-Bromosa1icy1a1dehydezpentane-1,3-diamine

12、,nicke1ch1oride,copperacetateandsodiumazidewerepurchasedfromSigmaA1drich.A11otherchemica1swerecommercia11yavai1ab1eandusedasreceived.E1ementa1ana1ysiswascarriedoutusingmode12400Perkin-E1merCHNana1yzer.Infraredspectrawereco11ectedbyusingKBrpe11etsonaJasco-5300FTIRspectrophotometer.E1ectronicspectrawe

13、recarriedoutwitha1AMBDA35spectrometer.SynthesisofH21.4-Bromosa1icy1a1dehyde(2.0g,10mmo1)wasdisso1vedin50m1methano1,towhichwasaddeds1ow1yamethano1icso1ution(30m1)ofpentane-1,3-diamine(0.49g,5.0mmo1)withcontinuousstirring.Themixturewasreactedunderref1uxfor30minandcoo1edtoroomtemperature.Aye11owpowderp

14、roductwasobtainedbyfi1tration.Theso1idwasre-crysta11izedfrommethano1togiveye11owcrysta11ineproduct.Yie1d:1.83g(81%).Ana1.ca1cdforCi8Hi8Br2N2O2(%):C47.60,H3.99,N6.17.Found(%):C47.45,H4.12,N6.08.IRdata(KBr;vmax,cm1):3417w,3019w,2930wz2892wz2858w,1632s,1510m,1413m,1336w,1285w,1209m,1145wz1108m,1031w,97

15、6m,900w,845sz798m,613w,545w,469w.UV-Visdatainmethano1(znm(z1Bmo唱CmT):275(3.530104),303(1.720104),381(2.1501O4).1HNMR(500MHz,d6-DMSO),ppm13.00(s,1H,OH),8.53(s,1H,CH=N)z8.51(s,1H,CH=N),7.37(d,2H,ArH),7.02(m,3H,ArH),6.90(d,1H,ArH),3.57(t,2H,CH2),3.29(t,1H,CH),1.98(m,2H,CH2),1.59(mz2H,CH2),0.83(t,3H,CH3

16、).13CNMR(126MHz,d6-DMSO)z,ppm165.54,164.40,163.44,162.82,133.22,133.18,125.94z125.76,120.96,120.59,119.96,119.70,117.34,117.27,67.23,54.27,35.71,28.35,10.17.Synthesisofcomp1ex1.H21(0.45g,1.0mmo1)wasdisso1vedinmethano1(30m1)ztowhichwasaddedamethano1icso1ution(15m1)ofnicke1ch1oridetetrahydrate(0.48g,2.0mmo1)withcontinuousstirring.Then,sodiumazide(0.13g,2.0mmo1)wasadded.Thefi