{"title":"2,4-二甲基-8-氢硒喹啉酸钯的合成与结构","authors":"E. Silina, S. Belyakov, A. Tokmakov, D. Zaruma","doi":"10.7250/MSAC.2013.008","DOIUrl":null,"url":null,"abstract":"The internal complex palladium 2,4-dimethyl-8- hydroselenoquinolinate Pd[C9H4(CH3)2NSe]2 (I) has been synthesized in the course of study of the complexing activity of 8- hydroselenoquinoline and investigation of the nature of chemical bond metal-selenium in the five-membered metal-containing ring. X-ray diffraction data for I: Monoclinic, space group P21/n, a = 9.0092(4), b = 16.3290(7), c = 14.1073(6) A, = 106.710(2)o, V = 1987.7(2) A3, Z = 4, R1=0.0477, wR2=0.1182 for 4499 reflections (diffractometer Bruker-Nonius KappaCCD, MoK). The crystal structure of the complex I is formed by neutral asymmetric molecules Pd[C9H4(CH3)2NSe]2 in which the central atom palladium is connected bidentically (Se,N) with two 2,4- dimethyl-8-hydroselenoquinoline ligands. The structure of palladium coordination polyhedron is cis-square (2Se+2N) somewhat tetrahedrally distorted. Dihedral angle between the SePdN / SePdN coordination planes is 20.15(1)o. The Pd–Se and Pd–N bonds are covalent. The transition of trans- (complex Pd(C9H6NSe)2 (II) to cis-coordination (complex I) causes the weakening of the Pd–N bonds (compare 2.162(5) and 2.159(5) A (I) , 2.065(3) A (II) ).","PeriodicalId":18239,"journal":{"name":"Materials Science and Applied Chemistry","volume":"30 1","pages":"45-50"},"PeriodicalIF":0.0000,"publicationDate":"2013-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"The Synthesis and Structure of Palladium 2,4-dimethyl-8-hydroselenoquinolinate\",\"authors\":\"E. Silina, S. Belyakov, A. Tokmakov, D. Zaruma\",\"doi\":\"10.7250/MSAC.2013.008\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"The internal complex palladium 2,4-dimethyl-8- hydroselenoquinolinate Pd[C9H4(CH3)2NSe]2 (I) has been synthesized in the course of study of the complexing activity of 8- hydroselenoquinoline and investigation of the nature of chemical bond metal-selenium in the five-membered metal-containing ring. X-ray diffraction data for I: Monoclinic, space group P21/n, a = 9.0092(4), b = 16.3290(7), c = 14.1073(6) A, = 106.710(2)o, V = 1987.7(2) A3, Z = 4, R1=0.0477, wR2=0.1182 for 4499 reflections (diffractometer Bruker-Nonius KappaCCD, MoK). The crystal structure of the complex I is formed by neutral asymmetric molecules Pd[C9H4(CH3)2NSe]2 in which the central atom palladium is connected bidentically (Se,N) with two 2,4- dimethyl-8-hydroselenoquinoline ligands. The structure of palladium coordination polyhedron is cis-square (2Se+2N) somewhat tetrahedrally distorted. Dihedral angle between the SePdN / SePdN coordination planes is 20.15(1)o. The Pd–Se and Pd–N bonds are covalent. The transition of trans- (complex Pd(C9H6NSe)2 (II) to cis-coordination (complex I) causes the weakening of the Pd–N bonds (compare 2.162(5) and 2.159(5) A (I) , 2.065(3) A (II) ).\",\"PeriodicalId\":18239,\"journal\":{\"name\":\"Materials Science and Applied Chemistry\",\"volume\":\"30 1\",\"pages\":\"45-50\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2013-10-18\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Materials Science and Applied Chemistry\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.7250/MSAC.2013.008\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Materials Science and Applied Chemistry","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.7250/MSAC.2013.008","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
摘要
通过对8-氢硒喹啉络合活性的研究和对五元含金属环中化学键金属-硒性质的研究,合成了内部配合物钯2,4-二甲基-8-氢硒喹啉酯Pd[C9H4(CH3)2NSe]2 (I)。x射线衍射数据I:单斜,空间群P21/n, a = 9.0092(4), b = 16.3290(7), c = 14.1073(6) a,= 106.710(2)o, V = 1987.7(2) A3, Z = 4, R1=0.0477, wR2=0.1182, 4499反射(衍射仪Bruker-Nonius KappaCCD,整机MoK)。配合物I的晶体结构是由中性不对称分子Pd[C9H4(CH3)2NSe]2形成的,其中中心原子钯与两个2,4-二甲基-8-氢硒喹啉配体双相连接(Se,N)。钯配位多面体的结构为顺方形(2Se+2N),有一定的四面体畸变。SePdN / SePdN配位面之间的二面角为20.15(1)0。Pd-Se和Pd-N键是共价的。反式(配合物Pd(C9H6NSe)2 (II)向顺式配位(配合物I)的转变导致Pd - n键减弱(比较2.162(5)和2.159(5)A (I), 2.065(3) A (II)))。
The Synthesis and Structure of Palladium 2,4-dimethyl-8-hydroselenoquinolinate
The internal complex palladium 2,4-dimethyl-8- hydroselenoquinolinate Pd[C9H4(CH3)2NSe]2 (I) has been synthesized in the course of study of the complexing activity of 8- hydroselenoquinoline and investigation of the nature of chemical bond metal-selenium in the five-membered metal-containing ring. X-ray diffraction data for I: Monoclinic, space group P21/n, a = 9.0092(4), b = 16.3290(7), c = 14.1073(6) A, = 106.710(2)o, V = 1987.7(2) A3, Z = 4, R1=0.0477, wR2=0.1182 for 4499 reflections (diffractometer Bruker-Nonius KappaCCD, MoK). The crystal structure of the complex I is formed by neutral asymmetric molecules Pd[C9H4(CH3)2NSe]2 in which the central atom palladium is connected bidentically (Se,N) with two 2,4- dimethyl-8-hydroselenoquinoline ligands. The structure of palladium coordination polyhedron is cis-square (2Se+2N) somewhat tetrahedrally distorted. Dihedral angle between the SePdN / SePdN coordination planes is 20.15(1)o. The Pd–Se and Pd–N bonds are covalent. The transition of trans- (complex Pd(C9H6NSe)2 (II) to cis-coordination (complex I) causes the weakening of the Pd–N bonds (compare 2.162(5) and 2.159(5) A (I) , 2.065(3) A (II) ).