Issue 18, 2011
From the journal:

Dalton Transactions

Synthesis, characterization, crystal structure and preliminary reactivity behaviour of new heteropolytopic ligands based on the 1,3,5-triazine spacer and pyrazolyl, tris-pyrazolylmethyl and tris-pyrazolylethoxy bonding fragments†

C. Di Nicola,a   F. Garau,b   F. Marchetti,a   M. Monari,*c   L. Pandolfo,*b   C. Pettinari*a  and  A. Venzod  

* Corresponding authors

a Dept. of Chemical Sciences, Via S. Agostino, 1, University of Camerino, Camerino, (MC), Italy
E-mail: claudio.pettinari@unicam.it
Fax: +39 0737 637345
Tel: +39 0737 402234

b Dept. of Chemical Sciences, University of Padova, Via Marzolo, 1, Padova, Italy
E-mail: luciano.pandolfo@unipd.it
Fax: +39 049 8275161
Tel: +39 049 8275157

c Dept. of Chemistry “G. Ciamician”, University of Bologna, Via Selmi, 2, Bologna, Italy
E-mail: magda.monari@unibo.it
Fax: +39 051 2099456
Tel: +39 051 2099559

d CNR – ISTM and INSTM, University of Padova, Via Marzolo, 1, Padova, Italy

Abstract

Four new potentially polytopic nitrogen donor ligands based on the 1,3,5-triazine fragment, L1–L4 (L1 = 2-chloro-4,6-di(1H-pyrazol-1-yl)-1,3,5-triazine, L2 = N,N′-bis(4,6-di(1H-pyrazol-1-yl)-1,3,5-triazin-2-yl)ethane-1,2-diamine, L3 = 2,4,6-tris(tri(1H-pyrazol-1-yl)methyl)-1,3,5-triazine, and L4 = 2,4,6-tris(2,2,2-tri(1H-pyrazol-1-yl)ethoxy)-1,3,5-triazine) have been synthesized and characterized. The X-ray crystal structure of L3 confirms that its molecular nature consists of a 1,3,5-triazine ring bearing three tripodal tris(pyrazolyl) arms. L1, L2, and L4 react with CuI, CuII, PdII and AgI salts yielding mono-, di-, and oligonuclear derivatives: [Cu(L1)(Cy3P)]ClO4, [{Ag2(L2)}(CF3SO3)2]·H2O, [Cu2(L2)(NO3)2](NO3)2·H2O, [Cu2(L2)(CH3COO)2](CH3COO)2·3H2O, [Pd2(L2)(Cl)4]·2H2O, [Ru(L2)(Cl)(OH)]·CH3OH, [Ag3(L4)2](CF3SO3)3 and [Ag3(L4)2](BF4)3. The interaction of L3 with AgI, CuII, ZnII and RuII complexes unexpectedly produced the hydrolysis of the ligand with formation, in all cases, of tris(pyrazolyl)methane (TPM) derivatives. In detail, the already known [Ag(TPM)2](CF3SO3) and [Cu(TPM)2](NO3)2, as well as the new [Zn(TPM)2](CF3SO3)2 and [Ru(TMP)(p-cymene)]Cl(OH)·2H2O complexes have been isolated. Single-crystal XRD determinations on the latter derivatives confirm their formulation, evidencing, for the RuII complex, an interesting supramolecular arrangement of the anions and crystallization water molecules.

Graphical abstract: Synthesis, characterization, crystal structure and preliminary reactivity behaviour of new heteropolytopic ligands based on the 1,3,5-triazine spacer and pyrazolyl, tris-pyrazolylmethyl and tris-pyrazolylethoxy bonding fragments

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Article information

DOI
https://doi.org/10.1039/C0DT01787F
Article type
Paper
Submitted
16 Dec 2010
Accepted
24 Feb 2011
First published
29 Mar 2011

Dalton Trans., 2011,40, 4941-4953

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Synthesis, characterization, crystal structure and preliminary reactivity behaviour of new heteropolytopic ligands based on the 1,3,5-triazine spacer and pyrazolyl, tris-pyrazolylmethyl and tris-pyrazolylethoxy bonding fragments

C. Di Nicola, F. Garau, F. Marchetti, M. Monari, L. Pandolfo, C. Pettinari and A. Venzo, Dalton Trans., 2011, 40, 4941 DOI: 10.1039/C0DT01787F

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