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Synthesis and Crystal Structure of Potassium Crown Ether Tetrathiosquarate

Synthesis and Crystal Structure of Potassium Crown Ether Tetrathiosquarate

作     者:Johannes Beck Younis O. Ben Amer 

作者机构:Institute of Inorganic Chemistry University of Bonn Bonn D-53121 Germany Department of Chemistry University of Garyounis Benghazi-Libya 

出 版 物:《Journal of Chemistry and Chemical Engineering》 (化学与化工(英文版))

年 卷 期:2012年第6卷第5期

页      面:470-474页

学科分类:081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070303[理学-有机化学] 0703[理学-化学] 070301[理学-无机化学] 

主  题:Tetrathiosquarate crown ether potassium ion complex formation crystal structure. 

摘      要:Slow diffusion of diethylether into a concentrated solution of K2C454.H20 and two equivalents of 18-crown-6 in pyridine affords dark orange crystals of bis(potassium{18-crown-6})(3-cyclobutene-1,2-dithione-3,4-dithiolate) [K(C12H2406)]2(CnS4). The crystal structure determination (monoclinic, P 2t/n, a = 12.2095(8) A, b = 11.3263(8) A, c = 14.0552(7) A, fl = 101.032(3)~, Z = 2) shows the presence of C4S42 - ions with almost undistorted D4h symmetry having C-C bond lengths of 1.442(10) A and 1.478(8) A and C-S bond lengths of 1.651(8) A and 1.664(7) A. Since the K+ ions are shielded in a half-spherical way by the crown ether ligands, the crystal structures is built of centrosymmetric molecular entities [(18-crown-6)K(C4S4)K(18-crown-6)]. The K+ ions have eight of coordination number, C4S42- acts as a chelating and bridging ligand towards two K+ with K-S distances of 3.434(2) A and 3.380(2) A.

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