Synthesis and crystal structures of ionic triphenyltin complexes with oxalic and malonic acid

被引:6
作者
Thorpe, Dain [1 ]
Callejas, Andrei [1 ]
Royzman, Dmitry [2 ]
Pike, Robert D. [2 ]
Eng, George [1 ]
Song, Xueqing [1 ]
机构
[1] Univ Dist Columbia, Dept Chem & Phys, Washington, DC USA
[2] Coll William & Mary, Dept Chem, Williamsburg, VA 23185 USA
基金
美国国家科学基金会;
关键词
Ionic; Triphenyltin; Hydrogen bonding; X-ray; DICARBOXYLIC-ACIDS; DIORGANOTIN(IV) COMPLEXES; ORGANOTIN CARBOXYLATES; CHEMISTRY; ESTERS; TIN; DINUCLEAR;
D O I
10.1080/00958972.2013.848275
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Two ionic triphenyltin complexes (1 and 2) were obtained via condensation of triphenyltin hydroxide with oxalic and malonic acids in the presence of di-isobutylamine. Their structures have been characterized by IR and multinuclear (H-1, C-13, and Sn-119) NMR spectroscopies. The coordinations of tin in the two triphenyltin complexes are confirmed by X-ray crystallographic studies. In the solid state, oxalate complex 1 consists of a di-isobutylammonium cation and an oxalatotriphenylstannate anion. Tin is five-coordinate with a cis-trigonal-bipyramid (TBP) geometry, as the oxalate is a chelating bidentate ligand. Complex 1 is a 1-D polymer via hydrogen bonding between carboxylate oxygen and ammonium nitrogen. The crystallographic studies reveal that 2 is a trinuclear triphenyltin complex formed with the molar ratio of tin, acid, and amine being 3:2:1. A negative charge is delocalized among the three tins in the complex; all tins have trans-TBP geometry with three phenyls in the equatorial plane and two O in axial positions. The malonates in 2 are bridging tridentate with the free carbonyl hydrogen bonded to di-isobutylammonium through an ethanol. This coordination and significant inter- and intramolecular hydrogen bonds between ammonium and malonate result in a 3-D polymeric structure for 2.
引用
收藏
页码:3647 / 3659
页数:13
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