First structurally characterized self-assembly of bipodal N-thiophosphorylated bis-thiourea with CoII: magnetic properties and thermal decomposition

Damir A. Safin; Maria G. Babashkina; Antoine P. Railliet; Nikolay A. Tumanov; Koen Robeyns; Eamonn Devlin; Yiannis Sanakis; Yaroslav Filinchuk; Yann Garcia

doi:10.1039/C3DT50254F

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Dalton Transactions

Issue 15, 2013

The international journal for inorganic, organometallic and bioinorganic chemistry

Impact Factor 3.838 48 Issues per Year Indexed in MEDLINE

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Paper

First structurally characterized self-assembly of bipodal N-thiophosphorylated bis-thiourea with Co^II: magnetic properties and thermal decomposition

Damir A. Safin,*^a Maria G. Babashkina,^a Antoine P. Railliet,^a Nikolay A. Tumanov,^a Koen Robeyns,^a Eamonn Devlin,^b Yiannis Sanakis,^b Yaroslav Filinchuk^a and Yann Garcia*^a

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Institute of Condensed Matter and Nanosciences, MOST – Inorganic Chemistry, Université Catholique de Louvain, Place L. Pasteur 1, 1348 Louvain-la-Neuve, Belgium
E-mail: damir.safin@ksu.ru ;
Fax: +32 (0) 1047 2330 ;
Tel: +32 (0) 1047 2831

Institute of Materials Science, NCSR Demokritos, Athens 15310, Greece

Dalton Trans., 2013,42, 5532-5538

DOI: 10.1039/C3DT50254F
Received 24 Jan 2013, Accepted 31 Jan 2013
First published online 31 Jan 2013

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Abstract
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Reaction of piperazine with isothiocyanate (iPrO)₂P(S)NCS leads to N-thiophosphorylated bis-thiourea (iPrO)₂P(S)NHC(S)NC₄H₈NC(S)NHP(S)(OiPr)₂ (H₂L). Recrystallization of H₂L from DMSO leads to the formation of the new ligand (iPrO)₂P(S)NC₄H₈NP(S)(OiPr)₂ (1). Reaction of doubly deprotonated L with Co^II leads to the [Co₂L₂] complex. The thermal properties of [Co₂L₂] in an air atmosphere were studied by means of TGA with the observed final residue corresponding to [CoPS₃]₂. The crystal structure of [Co₂L₂] was elucidated by single crystal X-ray diffraction. Two metal cations are in a tetrahedral 1,5-S₂S′₂ environment formed by the C [double bond, length as m-dash] S and PS sulfur atoms. Investigation of the temperature dependence of the magnetic susceptibility is consistent with two effectively non-interacting Co^II S = 3/2 ions.