Complexes [Ph3PR]2+[RuCl6]2−\documentclass[12pt]{minimal}
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\begin{document}$$\rm[{Ph_{3}PR]_2^+[RuCl_6]^{2-}}$$\end{document}, where R = C2H5 (I), CH=CHCH3 (II), CH2CH=CHCH3 (III), and CH2OCH3 (IV), have been prepared by the reaction between ruthenium(III) chloride hydrate and triphenylorganylphosphonium chlorides in dimethylsulfoxide in the presence of hydrochloric acid. A hydrochloric acid solution of ruthenium(III) chloride hydrate when mixed with an aqueous solution of 2-butylene-1,4- bis(triphenylphosphonium dichloride) followed by recrystallization from dimethylsulfoxide results in complex [Ph3PCH2CH=CHCH2PPh3]22+[Ru2Cl10O]4−\documentclass[12pt]{minimal}
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\begin{document}$$\rm[{Ph_{3}PCH_2CH=CHCH_2{PPh_3}]_2^{2+}[Ru_2Cl_{10}O]^{4-}}$$\end{document}· 4H2O (V). According to X-ray diffraction data, phosphorus atoms in mono- and binuclear cations have slightly distorted tetrahedral coordination (CPC 105.54(13)°−113.00(8)°, P−C 1.758(9)−1.839(7) Å). In slightly distorted octahedral anions [RuCl6]2− of complexes I–IV, the Ru−Cl bond lengths vary in the range 2.3222(6)−2.340(2) Å; the cis-ClRuCl and trans-ClRuCl angles are 89.133(18)°–90.867(18)° and 179.53(13)°–180°, respectively. In the binuclear [(RuCl5)2O]4− anion of complex V, RuCl5 fragments are bonded by a bridging oxygen atom. The Ru–Cl bond lengths fall in the range 2.3375(8)−2.3957(8) Å; the Ru–O bond length is 1.7832(2) Å. The cis-ClRuCl, trans-ClRuCl, cis-ORuCl, and trans-ORuCl angles are 86.67(3)°−91.28(3)°, 174.60(3)°−174.83(3)°, 91.49(2)°−93.65(2)°, and 178.39(2)°, respectively. In crystals I–V, interionic hydrogen bonds Cl···Hcation (2.63−2.95 Å), Cl··· HH2O\documentclass[12pt]{minimal}
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\begin{document}$${\rm{H}_{{H_2}O}}$$\end{document} (2.35−2.79 Å), and Hcation···OH2O\documentclass[12pt]{minimal}
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\begin{document}$${\rm{O}_{{H_2}O}}$$\end{document} (1.72−1.93 Å) (for V) are found.
