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Synthesis And Structure Of Complex With Schiff Base From Picolinaldehyde N-Oxide And Binuclear Mo(Ⅵ) Complex With Picolinato Ligands

Posted on:2002-03-22Degree:MasterType:Thesis
Country:ChinaCandidate:X B ChenFull Text:PDF
GTID:2121360032957207Subject:Inorganic Chemistry
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Copper(ll) complex [Cu(l-Ipiosn)(0N02)2] (1) was prepared from Cu(N03)e2H2O and N-oxide-2- formylpyridylsemicarbazone (H piosn) derived from the condensation reaction or the 2-forrnylpyri-dirie N-oxide and semicarbazone. The crystal stucture of )igand and compound had been determined by X-ray diffraction method,and crystalized in monoclinic.space groupP2 Ic, with unit cell parameters-:a=7.2685(8)A, b=8.748 1(7 ~1A, c= 13.9441(13) A,W886.64(15) A3 Z4, Dc= 1.485-mgcm3 , i0.1 18 mm',F(OOO)~4l6,-finaI R1=O.078. wR2=O.1803 s~1.2l5. X-ray single crystal diffraction studies of l-Ipiosii show that ~-dimensionaI network is formed through the strong hydrogen bonding between four Schiti' base molecules and one 1120 molecule. Compound belongs to monoclinic, space ~roupP21Ic, with unit cell parameters-:a=13.588(2) A,b=7.865(2)A, c=12.556(2) A,v=ii 1.110(10)A3 ,Z~4,Dc=1.9Sl mgA3, ~I.8O3mm', F(000)=740, final R1~O.O455, wR~~O.O86O s~O.99ü.The crystal structure of Compound indicates that its molecule structure adopts distorted square-pyramid geometry. The copper (II) center is five-coordinate and surrounded by t\~O oxygen atoms and one nitrogen atom from the neutral ligand Hpiosn, and two oxygen atoms from two nitrato groups, respectively. Two-dimensional network is formed via the strong inteimole-cular hydrogen bonding. The Iigand and complex are characterized by elemental analysis, IR and UV-vis spectrum.By the reaction of 2-formylpyridine N-oxide and phenyl hydrazine in the ethanol, NOxid-2-Formyl-pyridyl phenyl hydra.zine(b) was synthesized and its pale yellow single crystals was obtained. The crystal stuc-ture had been determined by X-ray diffraction method.Compond has the molecular formula C7H8N402H,0 andits crystal stucture belongs to monocli-nic,space groupP21/c, with unit cell parameters:a=7.2685(81A, b=8.7481 (2)A, c=]3.9441(2) A,V=886.64(10) A3 ,Z=4,-Dc~1.485 mgkt, k=O.l l8mni , F(000)=416, final R1=O.078.wR=O.1803,S=l.215. In crystal stucture of the compound(b)By hydrogen bonds(0( I) ~O(1W)2.719A , 0(1) ~"0(1Wa) 2.751 A) , Every 1-120 molecule interacts with ~ ligand(h molecule,which make net stucture of the compound.By the reaction of 2-formylpyridine N-oxide and 2-aminothiophenol in the eihanol, 2-picotinalde-hyde N-oxide 2-aminothiophenol was synthesized and itsdeep red singL crystals was obtained. The cry-stal stucture had been determined by X-ray diffraction nethod.Compond has the molecular formula C12H~N20S and its crystal stucturebJongs to monocli-nic,space groupP21/c,. with unit cell parameters: a=l I .938(2)A,b= 4.86 10-(lO)A, cl8.533(4)A, V=1033.8(4)A3 Z=4, Dc=l.467mgcm) , p.t=O.289mn1 F(0001= -472 ,final Rl-tJ.0446 , wR-~O.lO35. it-it stacking interaction exits in the crystal of the c&In-pound which make net stueture.By the reaction of salicylaldeliyde and 4-aminoaiitipyrine in the etl:mol. 4-salkylaldehydylamino-antipyrine was syn-thesized and its deep red single cry ials was obtained. The crystal stuclure had been determined by X-ray diffraction method.Con1ioiid has3the molecular formula C12H3N20S and its crystal stuc-ture belongs to monocli-nic,space group. P2,/c,. with unit cell parameters a=7.5970( I O)A-,b~7.5-00( 1 O)A,C=27.266(5)A, V=1546.7(4)A3 Z=4, Dc=l.320mgcm3 , ji=0.088mm' F(000)= 648 ,final Rl=0.0413. ~vR2=O.0952 Its spectroscopic properties had been studied by elec-tron spectrum,IR,'HN MR..At the commond condition, the reaction of picolinic acid and (n-Bu4N)Mo5026 in the CH~CN in the mole-cular ratio of l:l,binuclear molybdenum( VI) complex with picolinic was synthesized and at the same time its single crystals was obtained.The crystal structure had been determined by X-ray difTrac-tion method,and its spec-troscopic properties had been studied by IR, 'HNMR. Compond has the mole-cular formulal(n-Bu4N)2Mo2 (pic)2)and its crystal stucture belongs to monoclinic,space groupP2,/c, with unit cell parameters: a=9.941(2)A.b=13.719(2) A, c=18.824(2) A, p=l0O.840(l0)0, Mr=508.50, V=2521.4 (9) A3~3IDc=l.340-Mg/m , ~t=0.552mm , F (000) =1072. Co...
Keywords/Search Tags:2-picolinaldehyde N-oxide, semicarbazone, Schiff base, copper complex picolinic acid, binuclear molybdenum(Ⅵ) complex, crystal structure
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