The organometallic double metal cyanide [(Me-2 Sn)(3){Co(CN)(6)}(2)center dot 6H(2)O]. A three-dimensional framework of infinite, stapled ribbons

The admixture of aqueous Me2SnCl2-Me3SnCl solutions to solutions of K-3[Co( CN)(6)] in the molar ratios 3:0:2 and 1:1:1, respectively, affords precipit ates of [(Me2Sn)(3)(Co(CN)(6)}(2). 6H(2)O] (1) and [Me2Sn)(Me3Sn)Co(CN)(6)] (2). Another synthesis of 2 is based upon the bromination of [Me3Sn)(3)Co( CN)(6)] in MeOH. The crystal structure analysis of 1 reveals stacks of infi nite planar ribbons built up of trans-Me2Sn(mu-NC)(4) and trans-Me2Sn(mu-NC )(2)(OH2)(2) units as well as of trans-Co(CN)(2) fragments with terminal CN -ligands. Sn <-- OH2...(NC)(2) hydrogen bonds interlink adjacent ribbons. M ultinuclear (C-13, N-15, Co-59, Sn-119) CPMAS solid-state NMR studies of 1 suggest some intra-ribbon dynamics, and help in proposing both a plausible architecture for anhydrous 2 and a better understanding of the nature of an other precipitate 5 resulting from the admixture of a Me2SnCl2/ Me3SnCl sol ution to a solution of K-4[Fe(CN)(6)] (1:2:1). (C) 2000 Elsevier Science S. A. All rights reserved.