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Shane Ratcliffe - One of the best experts on this subject based on the ideXlab platform.
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the reactions of sbx3 x cl br i with n methylbenzothiazole 2 thione mbtt and n methylbenzothiazole 2 selone mbts formation of the mixed mer fac complex mer sbbr3 mbts 2 μ mbts fac sbbr3 mbts 2 ch2cl2
Polyhedron, 2010Co-Authors: Nicholas A Barnes, Stephen M Godfrey, Robin G Pritchard, Shane RatcliffeAbstract:Abstract The reactions of the Antimony(III) halides, SbX3 (X = Cl, Br, I) with the heterocyclic thione, N-methylbenzothiazole-2-thione (mbtt) and the analogous selone, N-methylbenzothiazole-2-selone (mbts) are reported. The products formed are highly dependent upon the identity of the halide, and in one case on the identity of the chalcogen donor Atom. The reaction of SbCl3 with both mbtt and mbts (and the reaction of SbBr3 with mbtt), forms complexes in CH2Cl2 with a 2:1 ligand to metal ratio, [SbX3(L)(μ-L)2SbX3(L)]·CH2Cl2, [X = Cl, L = mbtt (1), L = mbts (2); X = Br, L = mbtt (3)]. These complexes are weakly held together, and feature a primary pyramidal SbX3 coordination sphere with weak secondary donor-acceptor bonding to the chalcone donor ligands, giving an overall [3+3] octahedral geometry around each Antimony Atom. In contrast, the reaction of SbBr3 with mbts in CH2Cl2 produces a highly unusual 5:2 ligand:SbBr3 complex, [mer-SbBr3(mbts)2(-mbts)fac-SbBr3(mbts)2]·CH2Cl2 (4). The fac-substituted Antimony center has a [4+2] bonding arrangement, consisting of a primary [SbBr3(mbts)] coordination sphere and weaker secondary bonds to two further mbts ligands. In contrast, the bonding at the mer-substituted Antimony Atom is better described as [5+1], with a primary [SbBr3(mbts)2] coordination sphere and only one secondary bond to another mbts ligand. The complex is highly unusual in featuring two Antimony Atoms with different primary/secondary coordination spheres in the same complex. The reactions of mbtt and mbts with SbI3 result in the formation of 1:1 complexes [SbI3L], which display chain polymeric structures, {[SbI2(mbtt)(μ-I)]}n (5) and {[SbI2(mbts)(μ-I)]}n (6). The complexes consist of see–saw [SbI3L] units linked into polymeric chains by bridging iodine Atoms, the Antimony Atoms thus exhibits a square pyramidal geometry. The iodide complexes feature a stereochemically active lone pair trans to the apical iodine Atom, and feature much shorter Antimony–chalcogen bonds than observed for 1–4.
Nicholas A Barnes - One of the best experts on this subject based on the ideXlab platform.
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the reactions of sbx3 x cl br i with n methylbenzothiazole 2 thione mbtt and n methylbenzothiazole 2 selone mbts formation of the mixed mer fac complex mer sbbr3 mbts 2 μ mbts fac sbbr3 mbts 2 ch2cl2
Polyhedron, 2010Co-Authors: Nicholas A Barnes, Stephen M Godfrey, Robin G Pritchard, Shane RatcliffeAbstract:Abstract The reactions of the Antimony(III) halides, SbX3 (X = Cl, Br, I) with the heterocyclic thione, N-methylbenzothiazole-2-thione (mbtt) and the analogous selone, N-methylbenzothiazole-2-selone (mbts) are reported. The products formed are highly dependent upon the identity of the halide, and in one case on the identity of the chalcogen donor Atom. The reaction of SbCl3 with both mbtt and mbts (and the reaction of SbBr3 with mbtt), forms complexes in CH2Cl2 with a 2:1 ligand to metal ratio, [SbX3(L)(μ-L)2SbX3(L)]·CH2Cl2, [X = Cl, L = mbtt (1), L = mbts (2); X = Br, L = mbtt (3)]. These complexes are weakly held together, and feature a primary pyramidal SbX3 coordination sphere with weak secondary donor-acceptor bonding to the chalcone donor ligands, giving an overall [3+3] octahedral geometry around each Antimony Atom. In contrast, the reaction of SbBr3 with mbts in CH2Cl2 produces a highly unusual 5:2 ligand:SbBr3 complex, [mer-SbBr3(mbts)2(-mbts)fac-SbBr3(mbts)2]·CH2Cl2 (4). The fac-substituted Antimony center has a [4+2] bonding arrangement, consisting of a primary [SbBr3(mbts)] coordination sphere and weaker secondary bonds to two further mbts ligands. In contrast, the bonding at the mer-substituted Antimony Atom is better described as [5+1], with a primary [SbBr3(mbts)2] coordination sphere and only one secondary bond to another mbts ligand. The complex is highly unusual in featuring two Antimony Atoms with different primary/secondary coordination spheres in the same complex. The reactions of mbtt and mbts with SbI3 result in the formation of 1:1 complexes [SbI3L], which display chain polymeric structures, {[SbI2(mbtt)(μ-I)]}n (5) and {[SbI2(mbts)(μ-I)]}n (6). The complexes consist of see–saw [SbI3L] units linked into polymeric chains by bridging iodine Atoms, the Antimony Atoms thus exhibits a square pyramidal geometry. The iodide complexes feature a stereochemically active lone pair trans to the apical iodine Atom, and feature much shorter Antimony–chalcogen bonds than observed for 1–4.
Stephen M Godfrey - One of the best experts on this subject based on the ideXlab platform.
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the reactions of sbx3 x cl br i with n methylbenzothiazole 2 thione mbtt and n methylbenzothiazole 2 selone mbts formation of the mixed mer fac complex mer sbbr3 mbts 2 μ mbts fac sbbr3 mbts 2 ch2cl2
Polyhedron, 2010Co-Authors: Nicholas A Barnes, Stephen M Godfrey, Robin G Pritchard, Shane RatcliffeAbstract:Abstract The reactions of the Antimony(III) halides, SbX3 (X = Cl, Br, I) with the heterocyclic thione, N-methylbenzothiazole-2-thione (mbtt) and the analogous selone, N-methylbenzothiazole-2-selone (mbts) are reported. The products formed are highly dependent upon the identity of the halide, and in one case on the identity of the chalcogen donor Atom. The reaction of SbCl3 with both mbtt and mbts (and the reaction of SbBr3 with mbtt), forms complexes in CH2Cl2 with a 2:1 ligand to metal ratio, [SbX3(L)(μ-L)2SbX3(L)]·CH2Cl2, [X = Cl, L = mbtt (1), L = mbts (2); X = Br, L = mbtt (3)]. These complexes are weakly held together, and feature a primary pyramidal SbX3 coordination sphere with weak secondary donor-acceptor bonding to the chalcone donor ligands, giving an overall [3+3] octahedral geometry around each Antimony Atom. In contrast, the reaction of SbBr3 with mbts in CH2Cl2 produces a highly unusual 5:2 ligand:SbBr3 complex, [mer-SbBr3(mbts)2(-mbts)fac-SbBr3(mbts)2]·CH2Cl2 (4). The fac-substituted Antimony center has a [4+2] bonding arrangement, consisting of a primary [SbBr3(mbts)] coordination sphere and weaker secondary bonds to two further mbts ligands. In contrast, the bonding at the mer-substituted Antimony Atom is better described as [5+1], with a primary [SbBr3(mbts)2] coordination sphere and only one secondary bond to another mbts ligand. The complex is highly unusual in featuring two Antimony Atoms with different primary/secondary coordination spheres in the same complex. The reactions of mbtt and mbts with SbI3 result in the formation of 1:1 complexes [SbI3L], which display chain polymeric structures, {[SbI2(mbtt)(μ-I)]}n (5) and {[SbI2(mbts)(μ-I)]}n (6). The complexes consist of see–saw [SbI3L] units linked into polymeric chains by bridging iodine Atoms, the Antimony Atoms thus exhibits a square pyramidal geometry. The iodide complexes feature a stereochemically active lone pair trans to the apical iodine Atom, and feature much shorter Antimony–chalcogen bonds than observed for 1–4.
Robin G Pritchard - One of the best experts on this subject based on the ideXlab platform.
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the reactions of sbx3 x cl br i with n methylbenzothiazole 2 thione mbtt and n methylbenzothiazole 2 selone mbts formation of the mixed mer fac complex mer sbbr3 mbts 2 μ mbts fac sbbr3 mbts 2 ch2cl2
Polyhedron, 2010Co-Authors: Nicholas A Barnes, Stephen M Godfrey, Robin G Pritchard, Shane RatcliffeAbstract:Abstract The reactions of the Antimony(III) halides, SbX3 (X = Cl, Br, I) with the heterocyclic thione, N-methylbenzothiazole-2-thione (mbtt) and the analogous selone, N-methylbenzothiazole-2-selone (mbts) are reported. The products formed are highly dependent upon the identity of the halide, and in one case on the identity of the chalcogen donor Atom. The reaction of SbCl3 with both mbtt and mbts (and the reaction of SbBr3 with mbtt), forms complexes in CH2Cl2 with a 2:1 ligand to metal ratio, [SbX3(L)(μ-L)2SbX3(L)]·CH2Cl2, [X = Cl, L = mbtt (1), L = mbts (2); X = Br, L = mbtt (3)]. These complexes are weakly held together, and feature a primary pyramidal SbX3 coordination sphere with weak secondary donor-acceptor bonding to the chalcone donor ligands, giving an overall [3+3] octahedral geometry around each Antimony Atom. In contrast, the reaction of SbBr3 with mbts in CH2Cl2 produces a highly unusual 5:2 ligand:SbBr3 complex, [mer-SbBr3(mbts)2(-mbts)fac-SbBr3(mbts)2]·CH2Cl2 (4). The fac-substituted Antimony center has a [4+2] bonding arrangement, consisting of a primary [SbBr3(mbts)] coordination sphere and weaker secondary bonds to two further mbts ligands. In contrast, the bonding at the mer-substituted Antimony Atom is better described as [5+1], with a primary [SbBr3(mbts)2] coordination sphere and only one secondary bond to another mbts ligand. The complex is highly unusual in featuring two Antimony Atoms with different primary/secondary coordination spheres in the same complex. The reactions of mbtt and mbts with SbI3 result in the formation of 1:1 complexes [SbI3L], which display chain polymeric structures, {[SbI2(mbtt)(μ-I)]}n (5) and {[SbI2(mbts)(μ-I)]}n (6). The complexes consist of see–saw [SbI3L] units linked into polymeric chains by bridging iodine Atoms, the Antimony Atoms thus exhibits a square pyramidal geometry. The iodide complexes feature a stereochemically active lone pair trans to the apical iodine Atom, and feature much shorter Antimony–chalcogen bonds than observed for 1–4.
Шарутина, Ольга Константиновна - One of the best experts on this subject based on the ideXlab platform.
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Синтез и строение гидрата 2-[(6-аминопиримидин-4(3Н)-он-2-ил)сульфанил]ацетата тетрафенилсурьмы
Южно-Уральский государственный университет, 2019Co-Authors: Губанова, Юлия Олеговна, Шарутина, Ольга Константиновна, Ким, Дмитрий Гымнанович, Петрова, Ксения ЮрьевнаAbstract:TetraphenylAntimony 2-[(6-Aminopyrimidine-4(3H)-one-2-yl)sulfonyl]acetate, obtained due to substitution of the hydrogen Atom by the Ph4Sb-fragment in the carboxylic group, is a product of the reaction between pentaphenylAntimony and 2-[(6-aminopyrimidine-4(3H)-one-2-yl)sulfonyl]acetic acid. The compound has been isolated in the form of a hydrate with 78 % yield and represents colourless crystals with the melting point 197 °С. The compound has been characterized by IR-spectroscopy and X-ray analysis. The absorption bonds of the carbonyl groups in the cycle and acid fragment are present in the IR-spectra at the frequency 1629 and 1603 сm−1,respectively. According to the X-ray analysis, carried out on a D8 QUEST Bruker diffractometer, the compound unit cells parameters are: triclinic syngony, P group of symmetry; а = 9.551(3), b =13.469(3), c = 14.484(5) Å, α = 86.355(11)°, β = 74.421(18)°, γ = 76.483(10)°, V = 1745.0(9) Å3, ρcalc = 1.234 g/cm3. The Antimony Atom has a distorted trigonal bipyramidal coordination. The OSbC axial angle equals 179.42(10)°, the sum of angles in the equatorial plane equals 357.0(13)°. The Sb–C axial bond and equatorial bonds equal 2.175(3) Å and 2.107(3)−2.139(3) Å, respectively. The Sb−O bond length equals 2.253(2) Å. The single and double bond are not aligned (1.283(3) и 1.226(4) Å, respectively). The pyrimidine cycle is practically planar, the nitrogen and carbon Atoms deviate from the middle plane by no more than 0.012 Å; the sulfur Atom deviates from the middle plane by 0.106 Å.Продуктом взаимодействия пентафенилсурьмы с гидратом 2-[(6-аминопиримидин-4(3Н)-он-2-ил)сульфанил]уксусной кислоты является 2-[(6-аминопиримидин-4(3Н)-он- 2-ил)сульфанил]ацетат тетрафенилсурьмы, который образуется в результате замещения атома водорода на фрагмент Ph4Sb в карбоксильной группе. Соединение выделено в форме гидрата с выходом 78 % и представляет собой бесцветные кристаллы с температурой плавления 197 °С. Соединение охарактеризовано методами ИК-спектроскопии и рентгеноструктурного анализа. В ИК-спектре соединения имеются полосы поглощения карбонильных групп, находящихся в цикле и в кислотном остатке, с частотами 1629 и 1603 см−1 соответственно. По данным рентгеноструктурного анализа, проведенного на дифрактометре D8 QUEST фирмы Bruker, криталлографические параметры элементарной ячейки соединения: триклинная сингония, группа симметрии P ; а = 9,551(3), b = 13,469(3), c = 14,484(5) Å, α = 86,355(11)°, β = 74,421(18)°, γ = 76,483(10) °, V = 1745,0(9) Å3, ρвыч = 1,234 г/см3.Атом сурьмы имеет искаженную тригонально-бипирамидальную координацию. Аксиальный угол OSbC составляет 179,42(10)°, сумма углов в экваториальной плоскости равна 357,0(13)°. Аксиальная связь и экваториальные связи Sb–C равны 2,175(3) Å и 2,107(3)−2,139(3) Å соответственно. Длина связи Sb−O составляет 2,253(2) Å. В молекуле одинарная и двойная связи С−О в карбоксильной группе не выровнены (1,283(3) и 1,226(4) Å соответственно). Пиримидиновый цикл является практически плоским, атомы углерода и азота отклоняются от средней плоскости не более, чем на 0,012 Å; атом серы выходит из плоскости цикла на величину, равную 0,106 Å
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Синтез и строение cольвата 2,6-пиридиндикарбоксилата бис(тетрафенилсурьмы) с толуолом
Южно-Уральский государственный университет, 2019Co-Authors: Губанова, Юлия Олеговна, Шарутина, Ольга КонстантиновнаAbstract:At interaction of pentaphenylAntimony with 2,6-pyridinedicarboxylic acid (mole ratio 1:1 or 2:1) in a toluene solution, bis(tetraphenylAntimony) 2,6-pyridinedicarboxylate toluene solvate (1) has been obtained for the first time (yield 72%, colorless crystals, m.p. 170 °C). The compound 1 has been characterized by IR-spectroscopy, elemental and X-ray analysis. The absorption band of a carbonyl group with the frequency 1620 cm–1 is present in the IR-spectrum, shifting towards the area of low-frequency oscillations in comparison with the spectrum of the acid (1701 cm–1). According to the data of X-ray analysis the unit cell crystallographic parameters of compound 1: triclinic syngony, the symmetry group P; a = 12.494(5), b = 13.788(5); c = 16.684(6) Å; V = 2550.5(16) Å3; Z = 2; ρ(calc.) = 1.455 g/сm3. The Sb(1) and Sb(2) Atoms in a molecule have a distorted trigonal-bipyramidal coordination in different degrees. The CSb(1)O and CSb(2)O axial angles equal 178.41(10)° and 176.75(11)°, the CSb(1)C and CSb(2)C equatorial angles vary in the ranges 111.58(14)–125.24(13)°) and 103.44(13)−146.5(11)°. The Sb(1,2)−O bond lengths equal 2.301(2), 2.310(2) Å. The Sb(1,2)–Ceqv equatorial bonds (2.105(3)–2.112(3) Å and 2.140(3)–2.162(3) Å) are shorter than the Sb(1,2)–Cax axial one (2.177(3), 2.162(3) Å). The bidentate binding of carboxylate ligands is weak (the distance Sb(1)∙∙∙O(2) equals 3,263(4) Å) it has been proved by significant difference in the lengths of single (С–О 1.288(3), 1.261(4) Å) and double bonds (С=О 1.226(3), 1.236(4) Å) in the carboxylate groups. The pypidine ring nitrogen Atom coordinates to the Antimony Atom (the distance Sb(2)∙∙∙N equals 2.947(3) Å).Взаимодействием пентафенилсурьмы с 2,6-пиридиндикарбоновой кислотой (мольное соотношение 1:1 или 2:1) в растворе толуола с выходом 72 % впервые синтезирован сольват 2,6-пиридиндикарбоксилата бис(тетрафенилсурьмы) с толуолом (1), который представляет собой бесцветные кристаллы с температурой плавления 170 °С. Соединение охарактеризовано методами ИК-спектроскопии, элементного анализа, рентгеноструктурного анализа. В ИК-спектре имеется полоса поглощения карбонильной группы с частотой 1620 см−1,смещенная в область низкочастотных колебаний по сравнению с ИК-спектром исходной кислоты и справочным значением. По данным рентгеноструктурного анализа, криталлографические параметры элементарной ячейки соединения 1: триклинная сингония, группа симметрии P ; a = 12,494(5), b = 13,788(5); c = 16,684(6) Å; V = 2550.5(16) Å3; Z = 2; r(выч.) = 1,455 г/см3. В молекуле атомы сурьмы Sb(1) и Sb(2) имеют искаженную в различной степени тригонально-бипирамидальную координацию. Аксиальные углы CSb(1)O и CSb(2)O равны 178,41(10)° и 176,75(11)°, экваториальные углы CSb(1)C и CSb(2)C варьируют в интервалах 111,58(14)−125,24(13)°) и 103,44(13)−146,5(11)°. Длины связей Sb(1,2)−O составляют 2,301(2), 2,310(2) Å. Экваториальные связи Sb(1,2)−Cэкв (2,105(3)–2,112(3) Å и 2,140(3)−2,162(3) Å) короче, чем аксиальные связи Sb(1,2)−Cакс (2,177(3), 2,162(3) Å). Бидентатный характер связывания карбоксильных групп проявляется слабо (расстояние Sb(1)∙∙∙O(2) составляет 3,263(4) Å), что подтверждается существенной разницей в значениях одинарных (С−О 1,288(3), 1,261(4) Å) и двойных связей (С=О 1,226(3), 1,236(4) Å). Атом азота пиридинового кольца координирует на атом сурьмы (расcтояние Sb(2)∙∙∙N составляет 2,947(3) Å)
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Synthesis and Structure of TetraphenylAntimony β-Isatoximate
Южно-Уральский государственный университет, 2018Co-Authors: Артемьева, Екатерина Владимировна, Шарутина, Ольга КонстантиновнаAbstract:(β-Isatoximato)tetraphenylAntimony (1) was obtained by the reaction of pentaphenylAntimony with β-isatoxime. X-ray diffraction analysis showed that the Antimony Atom in complex 1 had distorted trigonal-bipyramidal coordination
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SYNTHESIS AND STRUCTURE OF BIS(4-BROMOPHENOXY)TRIPHENYLAntimony
Южно-Уральский государственный университет, 2016Co-Authors: Шарутин, Владимир Викторович, Шарутина, Ольга КонстантиновнаAbstract:Interaction of triphenylAntimony with 4-bromophenol in the presence of tert-butylhydroperoxide in ether has led to the synthesis of bis(4-bromophenoxy)triphenylAntimony, whose structure has been established by X-ray diffraction analysis. The Antimony Atom has distorted trigonal-bipyramidal coordination with aroxy groups in axial positions. The bond lengths equal: 2.094(4), 2.108(5), 2.109(5) Å for Sb–C; 2.062(4) and 2.066(3) Å for Sb-O. The axial angle OSbO equals 172.41(1)°
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СТРОЕНИЕ ДИБЕНЗОИЛМЕТАНАТА ТЕТРАФЕНИЛСУРЬМЫ. ФАКТОРЫ, ВЛИЯЮЩИЕ НА ПРОЧНОСТЬ СВЯЗЫВАНИЯ ЛИГАНДА В β-ДИКЕТОНАТНЫХ КОМПЛЕКСАХ СУРЬМЫ (V)
Южно-Уральский государственный университет, 2015Co-Authors: Шарутин, Владимир Викторович, Шарутина, Ольга КонстантиновнаAbstract:TetraphenylAntimony dibenzoylmethanate (1) was obtained by substitution reaction from pentaphenylAntimony and dibenzoylmethane (2) in toluene. The ligand is bidentate in molecule 1, Antimony Atom has octahedral coordination (trans-angles CSbO and CSbC 165.7(1)°, 168.7(1)° and 159.4(2)°, distances Sb–O 2.256(3), 2.235(3) Å, Sb–С 2.157(4)–2.170(4) Å). Compound 2 is in the enol form in the crystal, the length of C=O and O–C bonds are equal to 1.283(2) and 1.303(2) Å.Дибензоилметанат тетрафенилсурьмы (1) синтезирован по реакции замещения из пентафенилсурьмы и дибензоилметана (2) в толуоле. В молекуле 1 лиганд бидентатен, координация атома сурьмы октаэдрическая (транс-углы CSbO и CSbC 165,7(1)°, 168,7(1)° и 159,4(2)°, расстояния Sb–O 2,256(3), 2,235(3) Å, Sb–С 2,157(4)–2,170(4) Å). В кристалле соединение 2 находится в енольной форме, длины связей C=O и C–O равны 1,283(2) и 1,303(2) Å