Synthesis and Structures of Potassium and Rubidium Arenesulfonates

Brian J. Gunderman, Philip J. Squattrito

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Abstract

A series of potassium and rubidium salts of substituted benzenesulfonates have been prepared by reaction of the metal hydroxide and sulfonic acid or sulfonate salt in water or water-ethanol solution. The structures were determined by single-crystal X-ray diffraction techniques. Crystal data: K2(O2CC6H4SO3), orthorhombic, Pbca, a = 13.827(2) A,b = 7.088(2) Å, c = 20.536(2) Å, V= 2013(1) Å3, Z = 8, R(Fo) = 0.035 for 1382 observations (I> 3σ(I)), 137 variables; Rb0.81k1.19)(O2CC6H4SO3), orthorhombic, Pbca, a = 14.031(3) Å, b = 7.180(5) Å, c = 20.656(3) Å, V= 2081(1) Å3, Z = 8, R(Fo) = 0.040 for 686 observations (I> 3σ(I)), 138 variables; K(HO2CC6H4SO3)·2H2O, monoclinic, P21/a, a = 8.657(5) Å, b = 9.956(4) Å, c = 12.912(2) Å, β = 94.94(3)°, V = 1108.7(7) Å3, Z = 4, R(Fo) = 0.042 for 1228 observations (I> 3σ(I)), 146 variables; K3(H3C(H2N)C6H3SO3)3·3H2O, monoclinic, P21/a, a = 11.042(3) Å, b = 20.930(4) Å, c = 13.457(2) Å, β = 95.08(2)°, V= 3098(1) Å3, Z = 4, R(FÅo) = 0.043 for 2752 observations (I > 3 (I)), 379 variables; Rb(H3C(H2N)C6H3SO3), orthorhombic, Pbca, a = 10.977(4) Å, b = 7.670(3) Å, c = 22.591(3) Å, V= 1902(2) Å3, Z = 8,R(Fo) = 0.044 for 709 observations (I> 3σ(I)), 118 variables. All of the structures contain alternating layers of metal cations and sulfonate anions. There is direct bonding between the metal ion and the sulfonate oxygen atoms in each structure, with additional coordination to carboxylate, amine or water. The coordination numbers of the cations vary from six to eight and the geometries are irregular. The anhydrous dipotassium and mixed Rb-K 4-carboxybenzenesulfonate salts are isostructural while the monopotassium 4-carboxybenzenesulfonate dihydrate has a distinct structure. In the case of the 4-aminotoluene-2-sulfonate, the potassium and rubidium compounds have very different structures. The structures are compared with those of reported metal sulfonates and phosphonates in terms of the trends in coordination behavior of the metals towards the anions.

Original languageEnglish
Pages (from-to)2924-2931
Number of pages8
JournalInorganic Chemistry
Volume33
Issue number13
DOIs
StatePublished - Jun 1 1994

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