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Synthesis and structure of fluorinated tetraphenylantimony β-diketonates
Journal of Fluorine Chemistry ( IF 1.9 ) Pub Date : 2019-10-21 , DOI: 10.1016/j.jfluchem.2019.109393
Olga K. Sharutina , Vladimir V. Sharutin , Ekaterina V. Artem’eva , Daria M. Sopshina , Oleg S. Eltsov

The reactions of pentaphenylantimony with fluorinated β-diketones have been studied. The structure of the obtained compounds has been determined by the X-ray diffraction method and confirmed by IR, 1H, 13C and 19F NMR spectroscopy. According to X-ray diffraction analysis data, the reaction products are tetraphenylantimony 1,1,1-trifluoropentane-2,4-dionate (), 1,1,1-trifluoro-5,5-dimethylhexane-2,4-dionate (3b) and 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyloctane-3,5-dionate (3c): Ph4Sb[OC(R)CHC(R')O] (R = CH3 (3a), Bu-t (3b, 3c); R' = CF3 (3a, 3b), C3F7 (3c)), the antimony atoms in the molecules have a distorted octahedral coordination. The CSbC angles equal 158.26(14)°, 157.90(9)°, 157.75(15)° (3 ac), the CSbO angles are 164.70(12)°, 168.05(12)° (3a); 165.47(9)°, 167.37(7)° (3b); 164.96(14)°, 169.66(13)° (3c). The Sb–C bond lengths vary in the ranges of 2.142(4)–2.164(4) Å, 2.144(2)–2.160(2) Å, 2.142(4)–2.160(4) Å (3 ac), the Sb–O distances are 2.358(3), 2.333(3) Å (3a); 2.306(2), 2.339(2) Å (3b); 2.376(3), 2.289(3) Å (3c). The 3a and 3b 13C NMR spectra contain short spin-spin interactions between carbon and fluorine atoms with a large direct spin-spin coupling constant, 1JCF ≈ 286.0 Hz, which are characteristic for fluorinated compounds.



中文翻译:

氟化四苯基锑β-二酮酸酯的合成与结构

已经研究了五苯基锑与氟化β-二酮的反应。所获得的化合物的结构已经通过X射线衍射法确定并且通过IR,1 H,13 C和19 F NMR光谱法确认。根据X射线衍射分析数据,反应产物为四苯基1,1,1-三氟戊烷-2,4-二酸酯(),1,1,1-三氟-5,5-二甲基己烷-2,4-二酸酯(3b)和6,6,7,7,8,8,8-七氟-2,2-二甲基辛烷-3,5-二酸酯(3c):Ph 4 Sb [OC(R)CHC(R')O] (R = CH 3图3a),BU-图3b图3c); R'= CF 33a3b),C 3 F 73c)),分子中的锑原子具有扭曲的八面体配位。CSbC角等于158.26(14)°,157.90(9)°,157.75(15)°(3 ac),CSbO角分别为164.70(12)°,168.05(12)°(3a); 165.47(9)°,167.37(7)°(3b); 164.96(14)°,169.66(13)°(3c)。Sb–C键长在2.142(4)–2.164(4)Å,2.144(2)–2.160(2)Å,2.142(4)–2.160(4)Å(3 ac)的范围内变化, Sb-O距离为2.358(3),2.333(3)Å(3a);2.306(2),2.339(2)Å(3b); 2.376(3),2.289(3)Å(3c)。在图3a3b中 13 C NMR谱含有碳原子和氟原子之间的短的自旋-自旋相互作用的大的直接自旋-自旋耦合常数,1 Ĵ CF ≈286.0 Hz,这是氟化化合物的特性。

更新日期:2019-10-22
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