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µ 2 -Oxo-Bis[(2,5-Dinitrophenoxo)triarylantimony]: Syntheses, Structures, and Reactions with Pentaarylantimony
Russian Journal of Coordination Chemistry ( IF 1.9 ) Pub Date : 2020-03-18 , DOI: 10.1134/s1070328419120066
V. V. Sharutin , O. K. Sharutina , A. N. Efremov

Abstract

Antimony aroxides [Ph3SbOC6H3(NO2)2-2,5]2O (I) and [(4-MeC6H4)3SbOC6H3(NO2)2-2,5]2O (II) were synthesized by the oxidation of triarylantimony with tert-butyl hydroperoxide in the presence of 2,5-dinitrophenol. The SbOSb fragments in compounds I and II are bent (the corresponding angles are 139.70(10)° and 142.32(12)°). The Sb−Оbr bonds (1.973(3), 1.980(3) Å in I; 1.975(2), 1.977(2) Å in II) are substantially shorter than Sb−Ot (2.211(3), 2.213(3) and 2.191(2), 2.191(2) Å in I and II, respectively). Aroxides Ar4SbOC6H3(NO2)2-2,5 (Ar = Ph (III) and 4-MeC6H4 (IV)) and carbonates (Ar4Sb)2CO3 (Ar = Ph (V) and 4-MeC6H4 (VI)) are formed from Ar5Sb and compounds I and II in the presence of oxygen and carbon dioxide, respectively. In the trigonal bipyramidal molecules of compounds III and IV, the СSbO axial angles are 175.80(7)° and 176.86(10)° (Sb−O 2.290(2) and 2.342(2) Å, respectively). One of the antimony atoms in compound V and in crystallographically independent molecules of two types of compound VI is pentacoordinated (the Sb−Oax bond is 2.245(6) Å in V and is 2.263(3) and 2.263(3) Å in VIа and VIb, respectively), whereas the second antimony atom is hexacoordinated (Sb−O 2.249(6) and 2.273(5) Å in V; 2.216(2), 2.251(2) Å and 2.217(2), 2.251(2) Å in VIа and VIb). The crystallographic data are deposited with the Cambridge Crystallographic Data Centre (СIF files ССDС nos. 1890704 (I), 1890706 (II), 1890713 (III), 1890714 (IV), 994519 (V), and 994177 (VI)).


中文翻译:

µ 2 -Oxo-Bis [(2,5-Dinitrophenoxo)triaryl锑]:与五芳基锑的合成,结构和反应

摘要

氧化锑[Ph 3 SbOC 6 H 3(NO 22 -2,5] 2 O(I)和[(4-MeC 6 H 43 SbOC 6 H 3(NO 22 -2,5] 2 O(II)通过在2,5-二硝基苯酚存在下用丁基氢过氧化氧化三芳基锑合成。将化合物III中的SbOSb片段弯曲(相应的角度为139.70(10)°和142.32(12)°)。将SB-О BR键(I中的1.739(3),1.980(3)Å ; II中的1.975(2),1.977(2)Å )明显短于Sb-O t(2.211(3),2.213(3)和2.191(2 ),分别位于III中的2.191(2)Å )。氧化物Ar 4 SbOC 6 H 3(NO 22 -2,5(Ar = Ph(III)和4-MeC 6 H 4IV))和碳酸盐(Ar 4 Sb)2 CO 3(Ar = Ph(V)和4-MeC 6 H 4VI))分别由Ar 5 Sb和化合物III在氧气和二氧化碳存在下形成。在化合物IIIIV的三角双锥体分子中,СSbO轴向角为175.80(7)°和176.86(10)°(分别为Sb-O 2.290(2)和2.342(2)Å)。一个在化合物中的锑原子的V和在两种类型的化合物的结晶学上独立的分子VI是五配位的(Sb的-O键是2.245(6)在V和是2.263(3)和2.263(3)在VIаVIb),而第二个锑原子是六配位的(V中的Sb-O 2.249(6)和2.273(5)Å; V中的2.216(2),2.251(2)Å和2.217(2),2.251(2)Å VIаVIb)。晶体学数据存放在剑桥晶体学数据中心(СIF文件СD编号1890704(I),1890706(II),1890713(III),1890714(IV),994519(V)和994177(VI))。
更新日期:2020-03-18
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