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Synthesis, Characterization And Crystal Structures Of The Complexes With 2-mercapto Ethanesulfonic Acid

Posted on:2009-06-18Degree:MasterType:Thesis
Country:ChinaCandidate:X L HuFull Text:PDF
GTID:2121360245459546Subject:Inorganic Chemistry
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We have studied complex within Taurine for a long time in our lab,so have a good knowledge of its coordination chemistry. The mercapto is similar with the amido in the coordination ability, so we may compare the differrence.between them. And we can also find out some laws as well as expect to acquire some model complexes. At the same time , wo compare the distinetions between the carboxyl to the sulfonic,too.In order to systematically investigate the diversity of 2-mercapto ethanesulfonic acid and 2-mercapto acetic acid, then find out some laws as well as expect to acquire some model complexes, seven polymers was synthesized based on the previous studies together with more than one year's investigation. They are listed as follows.we choose the 2-mercapto ethanesulfonic acid ligand interacting with metal ions as our research subject. four novel complexes were synthesized.1. The reaction of 2-mercapto ethanesulfonic acid sodium salt and CuNO3·3H2O by entering the 1,3-D(4-pyridyl)propane as the reducing agent in presence of water produces a novel 12 nucleus copper cluster compound [Cu12L6(H2O)3]n(1). The crystal structure of complex (1) belongs to monoclinic, space group P2(1)/c with unit cell parameters: a = 11.8760(10) A, b = 17.6859(14) A, c = 18.9431(15) A,β= 96.9670(10) o, V = 3949.4(6) A3, Z = 2.2. The reaction of 2-mercapto ethanesulfonic acid sodium salt and Co(NO3)2·6H2O with 4,4'-bipy as coligand in water solution produces a 1D chains coordination polymer [Co (4,4'-bipy)3(H2O)3]n·2nL·2nH2O (2). Complex (2) crystallizes in triclinic, space group P1 with unit cell parameters: a = 11.4155(12) A, b = 13.1239(13) A, c = 5.4746(16) A,β= 76.6380(10)o, V = 2108.0(4) A3, Z = 2.3.A 2D layer coordination polymer [Ni2 (4,4'-bipy)3.5 6H2O]n·3nL·nClO4·3.5nH2O(3) was synthesized by reaction of 2-mercapto ethanesulfonic acid sodium salt and NiClO4·6H2O in water solvent. The X-ray crystallographic analysis indicates that the complex (3) crystallizes in monoclinic, space group P2/c with unit cell parameters: a = 22.457(2) A, b = 15.9613(14) A, c = 16.4147(15)A,β= 97.0710(10)o, V = 5839.0(9) A3, Z = 2。4. The reaction of 2-mercapto ethanesulfonic acid sodium salt and CuNO3·3H2O with 2,2'-bipy and 4,4'-bipy as coligand in water solution obtains a 1D infinite linear chain coordination polymer [Cu(4,4'-bipy)(2,2'-bipy)]n·2nL·nH2O (4). The results of X-ray crystallographic analysis indicates that complex (4) crystallizes in monoclinic, space group P2(1)/c with unit cell parameters: a = 8.385(2)A, b = 13.764(3)A, c = 21.719(5) A,β= 93.391(3) o, V = 2502.3(10) A3.we choose the 2-mercapto acetic acid ligand interacting with metal ions as our research subject. A novel complexes were synthesized. At the same time, two accessory production were synthesized, too.5. The reaction of 2-mercapto acetic acid and Co(NO3)2·6H2O with 4,4'-bipy as coligand and KOH adjusting the pH in methanol-water mixed solution acquire a new 2D rectangle latticework coordination polymer [CoL2(4,4'-bipy)]n(5)。Complex (5) belongs to triclinic, space group P1with unit cell parameters: a = 8.3038(11) A, b = 10.1549(13) A, c = 10.690(2) A,β= 98.452(2) o, V = 751.2(2) A3, Z = 2.6. (IV) The 1D chains coordination polymer [Cu2K(2,2'-bipy)2oxCl3]n·0.5nCuCl2(6) was synthesized by the diffuse treatment with K2C2O4·H2O, CuCl2 and the 4,4'-bipy as coligand in methanol and water solution. The results of X-ray crystallographic analysis indicate that the complex (6) belongs to triclinic, space group P1with unit cell parameters: a = 10.679(3) A, b = 10.728(3) A, c = 12.822(3) A,β= 111.021(3) o, V = 1322.2(6)A3.(IV) A 3D coordination polymer [CuSO4 (4,4'-bipy)(H2O)2]n·2nH2O(7) was synthesized by reaction of 4,4'-bipy and CuSO4·5H2O by the diffuseness in methanol-water solvent. The X-ray crystallographic analysis indicate that the complex (7) crystallizes in triclinic, space group Cc with unit cell parameters: a = 10.007(2) A, b = 19.841(4) A, c = 7.3878(15)A,β= 95.345(2) o, V = 1460.4(5) A3, Z = 4.In this paper, we synthesized seven coordination polymers which are not reported by the literature. They were characterized by the element analyse, IR and the X- crystallographic. We find that the mercapto is easy to form the complex with the transition metals. But the mercapto is also easily oxidated. It should pay attention to be protected.
Keywords/Search Tags:mercapto, 2-mercapto ethanesulfonic acid, coordination polymer, crystal structure
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