Intermolecular hydrogen-bonding in the solid-state structure of CpFe(CN)2(PTAH) Structural and spectral comparisons with its [K][CpFe(CN)2PTA] salt
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The salt K[CpFe(CN)2PTA] (1) has been synthesized from the photolysis of K[CpFe(CN)2CO] and 1,3,5-triaza-7-phosphaadamantane (PTA) in methanol. Protonation of the salt by hydrogen ion exchange employing DOWEX 50 WX8-100 ion exchange resin yielded the complex CpFe(CN)2PTAH (2). The solid-state structures of both compounds have been determined by X-ray crystallography. Protonation was shown via v(CN) and 31P-NMR to occur at one of the PTA nitrogens. Furthermore, it was found in the solid-state of the protonated structure that intermolecular hydrogen-bonding occurs between the cyanide nitrogen of one molecule and the PTA nitrogen of another molecule. The average Fe-CCN distance for 1 is 1.877(11) Å . Fe-CCN distances for complex 2 differ significantly at 1.839(12) and 1.940(12) Å , with the shorter bond length associated with the hydrogen-bonded CN group. Spectral (v(CN) and 31P-NMR) characterization of the complexes and their potential use as precursors to double metal cyanide derivatives are reported. © 2002 Elsevier Science B.V. All rights reserved.
author list (cited authors)
Darensbourg, D. J., Phelps, A. L., Adams, M. J., & Yarbrough, J. C.