Abstract

The crystal structure of [(nBu 4N){(Me 3Sn) 2OH}{Ni(CN) 4}][Ni(CN) 2 · 2Me 3SnCN · (nBu 4N)OH] ( 1), the formal 1:1-addition product of polymeric [(Me 3Sn) 2Ni(CN) 4][Ni(CN) 2 · 2Me 3SnCN] and (nBu 4N)OH, has been revisited at 153 K. Owing to the presence of distinct (Me 3Sn) 2OH · · ·NC hydrogen bonds, infinite, negatively charged layers containing cyclic [{(Me 3Sn) 2OH} 2{μ(NC) 2Ni(CN) 2} 2] 2− units alternate with layers of nBu 4N + ions. CPMAS solid-state NMR spectra ( 13C, 15N, 119Sn) strongly support nonsymmetric building blocks with exceedingly weak SnN bonds.

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