The One Stage Synthesis and Crystal Structure of 5,5,5-Trifluoro-2-pentanone-4,4-diolato-triphenylantimony(V)

被引:4
作者
Gushchin, Aleksey V. [1 ]
Usyatinsky, Rafail I. [1 ]
Fukin, Georgy K. [2 ]
Dodonov, Victor A. [1 ]
Zakharov, Lev N. [2 ]
机构
[1] Nizhnii Novgorod State Univ, Dept Organ Chem, Nizhnii Novgorod 603600, Russia
[2] Russian Acad Sci, GA Razuvaev Inst Organometall Chem, Nizhnii Novgorod 603600, Russia
关键词
D O I
10.1080/10241229812331341349
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
5,5,5-Trifluoro-2-pentanone-4,4-diolato-triphenylantimony((V)) was obtained by the one-step oxidation reaction of triphenylantimony, tert-butylhydroperoxide, and trifluoroacetylacetone. The crystal structure of 1 has been determined by X-ray diffraction method (MoK alpha-radiation, graphite monochromator, theta/2 theta-scan mode in the range 2 degrees <= 2 theta <= 54 degrees, 3734 observed reflection with F > 6 sigma(F), R = (0.029, Rw = 0.031, S = 1.03). Crystal of 1 is monoclinic, at 20 degrees C a = 9.369(5) angstrom, b = 16.891(6) angstrom, c = 13.934(5) angstrom, beta = 102.04(2)degrees, V = 2157(3) angstrom(3), d(calcd) = 1.611 g cm(-3), Z = 4, space group P2(1)/n. It was shown that 1 is a six-coordinated antimony complex. The coordination mode of the Sb atom in 1 can be described as a significantly distorted octahedron. In crystal structure the molecules of 1 are associated into a centro-symmetrical dimer by a weak hydrogen O center dot center dot center dot H-C bonds between adjacent molecules.
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页码:187 / 190
页数:4
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