2,4-二甲基-8-氢硒喹啉酸钯的合成与结构

E. Silina, S. Belyakov, A. Tokmakov, D. Zaruma
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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)))。
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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) ).
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