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Синтез и строение бис(2,5-диметилбензолсульфоната) и бис(дибромфторацетата) трис(3-фторфенил)сурьмы

Authors: Senchurin, V.S.; Filimonova, D.M.; Khromenko, V.E.;

Синтез и строение бис(2,5-диметилбензолсульфоната) и бис(дибромфторацетата) трис(3-фторфенил)сурьмы

Abstract

Сенчурин Владислав Станиславович – доктор химических наук, профессор, кафедра теоретической и прикладной химии, Южно-Уральский государственный университет. 454080, г. Челябинск, проспект Ленина, 76. E-mail: senchurinvs@susu.ru. Филимонова Дарья Михайловна – студент, Южно-Уральский государственный университет. 454080, г. Челябинск, проспект Ленина, 76. E-mail: rey.sammy@bk.ru. Хроменко Виктория Евгеньевна – студент, Южно-Уральский государственный университет. 454080, г. Челябинск, проспект Ленина, 76. E-mail: V.E.Hromenko@yandex.ru. V.S. Senchurin, senchurinvs@susu.ru D.M. Filimonova, rey.sammy@bk.ru V.E. Khromenko, V.E.Hromenko@yandex.ru South Ural State University, Chelyabinsk, Russian Federation Взаимодействием трис(3-фторфенил)сурьмы с 2,5-диметилбензолсульфоновой и дибромфторуксусной кислотами в присутствии трет-бутилгидропероксида (1:2:1 мольн.) получены бис(2,5-диметилбензолсульфонат) трис(3-фторфенил)сурьмы (1) и бис(дибромфторацетат) трис(3-фторфенил)сурьмы (2). По данным рентгеноструктурного анализа, проведенного при 293 К на автоматическом четырехкружном дифрактометре D8 Quest Bruker (двухкоординатный CCD – детектор, МоКα-излучение, λ = 0,71073 Å, графитовый монохроматор) кристаллов 1 [C34H30F2O6S2Sb, M 777,45; сингония триклинная, группа симметрии P–1; параметры ячейки: a = 10,634(18), b = 11,38(2), c = 14,31(3) Å; α = 90,51(8) град., β = 90,35(11) град., γ = 112,79(5) град.; V = 1596(5) Å3; размер кристалла 0,5 × 0,48 × 0,17 мм; интервалы индексов отражений –15 ≤ h ≤ 14, –15 ≤ k ≤ 15, –19 ≤ l ≤ 19; всего отражений 30473; независимых отражений 8318; Rint 0,0920; GOOF 1,894; R1 = 0,1699, wR2 = 0,4237; остаточная электронная плотность 6,78/–5,48 e/Å3] и 2 [C22H12O4F7SbBr2, M 754,89; сингония триклинная, группа симметрии P–1; параметры ячейки: a = 8,98(3), b = 10,41(2), c = 14,92(3) Å; α = 90,77(7) град., β = 90,73(9) град., γ = 113,95(10) град.; V = 1275(5) Å3; размер кристалла 0,65 × 0,32 × 0,14 мм; интервалы индексов отражений –13 ≤ h ≤ 13, –15 ≤ k ≤ 14, –21 ≤ l ≤ 21; всего отражений 61066; независимых отражений 8511; Rint 0,0863; GOOF 1,983; R1 = 0,1529, wR2 = 0,4647; остаточная электронная плотность 4,41/–3,48 e/Å3] атомы Sb имеют искаженную тригонально-бипирамидальную координацию. Аксиальные углы OSbO равны 178,2(3) (1) и 174,0(4) (2); сумма углов CSbC в экваториальной плоскости 360. Длины связей Sb–O 2,108(9), 2,111(8) Å (1) и 2,124(12), 2,131(12) Å (2); интервалы изменения длин связей Sb–C состав-ляют 2,090(11)–2,21(3) Å и 2,090(14)–2,096(16) Å. Структурная организация в кристаллах 1 и 2 обусловлена слабыми водородными связями типа O···H 2,53–2,70 Å (1) и 2,57–2,60 Å (2), F···H 2,46–2,59 Å (1) и Br···H 3,02 Å (2). В 2 также наблюдаются короткие контакты C···F между арильными лигандами соседних молекул 3,079 и 3,085 Å. Полные таблицы координат атомов, длин связей и валентных углов для структур 1 и 2 депонированы в Кембриджском банке структурных данных (№ 2055553, 2055764; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk). The interaction of tris(3-fluorophenyl)antimony with 2,5-dimethylbenzenesulfonic or di-bromofluoroacetic acid in diethyl ether in the presence of tert-butyl hydroperoxide has synthe-sized tris(3-fluorophenyl)antimony bis(2,5-dimethylbenzenesulfonate) (1) and tris(3-fluorophenyl)antimony bis(dibromofluoroacetate) (2). The X-ray diffraction pattern has been ob-tained at 293 K on an automatic diffractometer D8 Quest Bruker (MoKα-radiation, λ = 0.71073 Å, graphite monochromator) for crystal 1 [C34H30F2O6S2Sb, M 777.45, the triclinic syngony, the symmetry group P–1; cell parameters: a 10.634(18) Å, b 11.38(2) Å, c 14.31(3) Å, α = 90.51(8) degrees, β = 90.35(11) degrees, γ = 112.79(5) degrees; V = 1596(5) Å3; the crystal size is 0.5×0.48×0.17 mm; intervals of reflection indexes are –15 ≤ h ≤ 14, –15 ≤ k ≤ 15, –19 ≤ l ≤ 19; total reflections 30473; independent reflections 8318; Rint 0.0920; GOOF 1.894; R1 = 0.1699, wR2 = 0.4237; residual electron density 6.78/–5.48 e/Å3] and crystal 2 [C22H12O4F7SbBr2, M 754.89, the triclinic syngony, the symmetry group P–1; cell parameters: a 8.98(3) Å, b 10.41(2) Å, c 14.92(3) Å, α = 90.77(7) degrees, β = 90.73(9) degrees, γ = 113.95(10) degrees; V = 1275(5) Å3; the crystal size is 0.65 × 0.32 × 0.14 mm; intervals of reflection indexes are –13 ≤ h ≤ 13, –15 ≤ k ≤ 14, –21 ≤ l ≤ 21; total reflections 61066; independent reflections 8511; Rint 0.0863; GOOF 1.983; R1 = 0.1529, wR2 = 0.4647; residual electron density 4.41/–3.48 e/Å3] the antimony atoms have a distorted trigonal-bipyramidal coordination. The axial OSbO angles are 178.2(3) (1) and 174.0(4) (2); the sum of the CSbC angles in the equatorial plane is 360. The Sb–O and Sb–C bond lengths are 2.108(9)–2.131(12) Å and 2.090(14)– 2.21(3) Å. The struc-tural organization of crystals 1 and 2 is controlled by intermolecular bonds O···H 2.53–2.70 Å (1) and 2.57–2.60 Å (2), F···H 2.46–2.59 Å (1) and Br···H 3.02 Å (2). In 2 the short contacts C··· F have been observed between the aryl ligands of neighboring molecules 3.079 and 3.085 Å. Complete tables of coordinates of atoms, bond lengths and valence angles for structures 1 and 2 are deposited at the Cambridge Structural Data Bank (no. 2055553, 2055764; depo-sit@ccdc.cam.ac.uk; http: //www.ccdc.cam.ac.uk).

Country
Russian Federation
Keywords

рентгеноструктурный анализ, synthesis, УДК 546.863, 2,5-dimethylbenzenesulfonic acid, УДК 546.865, 2,5-диметилбензолсульфоновая кислота, синтез, УДК 548.312.5, дибромфторуксусная кислота, трис(3-фторфенил)сурьма, dibromofluo-roacetic acid, structure, строение, tris(3-fluorophenyl)antimony, УДК 547.53.024, X-ray analysis

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This is an alternative to the "Influence" indicator, which also reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
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popularity
This indicator reflects the "current" impact/attention (the "hype") of an article in the research community at large, based on the underlying citation network.
BIP!Popularity provided by BIP!
influence
This indicator reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
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impulse
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