Issue 7, 2002
From the journal:

New Journal of Chemistry

Synthesis and structure of phases containing [Ni3P3S12]3− crown-shaped trimers

Martine Bujoli-Doeuff,a   Servane Coste,a   Michel Evain,a   Raymond Brec,a   Dominique Massiotb  and  Stéphane Jobic*a  

* Corresponding authors

a Laboratoire de Chimie des Solides, Institut des Matériaux Jean-Rouxel, (CNRS UMR 6502) 2 rue de la Houssinière, BP 32229, Nantes cedex 3, France
E-mail: joloic@cnrs-imn.fr
Fax: +33 2 40 37 39 95
Tel: +33 2 40 37 39 17

b Centre de Recherches sur la Physique des Hautes Températures, (CNRS UPR 4212) 1D Avenue de la Recherche Scientifique, Orléans cedex 02, France
E-mail: massiot@cnrs-orleans.fr

Abstract

The exfoliation process of one-dimensional KNiPS4 showed that the breaking of 1/∞[NiPS4]− chains in polar solvent was followed by the formation of cyclic [Ni3P3S12]3− trianions. From DMF–KNiPS4 solutions, metathesis experiments were successfully carried out, but, up to now, K+ had only been exchanged by bigger isotropic organic cations such as PPh4+, (CH3)4N+ and (C2H5)4N+. After recrystallization, each metathesis compound presents the cyclic [Ni3P3S12]3− trianion. An exchange by anisotropic cations is possible by adding a cryptand molecule that fits the size of K+. Following this procedure, three new nickel thiophosphate complexes have been synthesized: [Ni3P3S12][K-(222-cryptand)]3 (I), [Ni3P3S12][K(222-cryptand)]2[C9N1H22] (II) and [Ni3P3S12][CH3(CH2)11N(CH3)3]3 (III). The structures of I and II have been fully determined from single crystal X-ray diffraction analysis. They show the occurrence of the [Ni3P3S12]3− trimer within the solid. I and II crystallize in the P212121 space group. 31P solid state NMR experiments hint at the presence of polyanions in III, maybe trianionic in nature.

Graphical abstract: Synthesis and structure of phases containing [Ni3P3S12]3− crown-shaped trimers

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Article information

DOI
https://doi.org/10.1039/B200703G
Article type
Paper
Submitted
18 Jan 2002
Accepted
13 Mar 2002
First published
25 Jun 2002

New J. Chem., 2002,26, 910-914

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Synthesis and structure of phases containing [Ni3P3S12]3− crown-shaped trimers

M. Bujoli-Doeuff, S. Coste, M. Evain, R. Brec, D. Massiot and S. Jobic, New J. Chem., 2002, 26, 910 DOI: 10.1039/B200703G

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