Structural characterization of [Crypt221-Na] 2 [H 2Ru 4 (CO) 12][Crypt222-K] 2 [Ru 4 (CO) 13

Abstract

The structures of [Crypt221-Na] 2 [H 2Ru 4 (CO) 12] and [Crypt222-K] 2 [Ru 4 (CO) 13] weredetermined from single crystal X-ray diffraction studies. A survey of the structures of tetranuclearcarbonyl clusters of the Group 8 metals and their conjugate bases is presented. The cluster core of [H 2Ru 4 (CO) 12] 2− is a tetrahedron of Ru atomswith three edge bridging carbonyls arranged around the base. Two single edge bridging hydrogensreside between the apical Ru atom and two basal Ru atoms. Two terminal carbonyls are bound toeach basal Ru atom and three terminal carbonyls are bound to the apical Ru atom. The apical Ruatom has three terminal carbonyls bound to it. In addition, two singly bridging hydrogens occurbetween apical and basal rutheniums. The [Ru 4 (CO) 13] 2−dianion structure consists of a tetrahedral Ru 4 core with three edge bridging carbonylsarranged around the base. Two semi-edge bridging carbonyls reside between the apical and twobasal Ru atoms. Crystal data for [Crypt221-Na] 2 [H 2Ru 4 (CO) 12] : space group P1̄, a = 13.718 (2) d , b = 20.997 (6) d , c = 10.344 (1) d , α = 97.02 (2) °, β = 92.81 (1) °, γ = 77.80 (2) °, V = 2889.56 d 3. Crystal datafor [Crypt222-K] 2 [Ru 4 (CO) 13] : space group P2 1/ c, a = 11.221 (3) d , b = 22.951 (6) d , c = 25.219 (6) d , β = 97.61 (2) °, V = 6427.74 d 3. © 1998 ElsevierScience Ltd. All rights reserved