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Synthesis, structural, and spectroscopic study of rhenium(III) and rhenium(V) 4,6-dimethylpyrimidine-2-thiolate/triphenylphosphine mixed complexes: Crystal and molecular structure of ∥ReCl2(pymS)(PPh3)2∥·C3H6O and ∥ReOCl2(pymS)(PPh3)∥

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Abstract

4,6-dimethylpyrimidine-2(1H)-thione reacts with rhenium(V) precursorstrans-∥ReOX3(PPh3)2∥ (X=Cl, Br) in acetone, to afford two classes of crystalline pyrimidinethiolate/triphenylphosphine mixed complexes:trans-∥ReIIIX2(C6H7N2S)(PPh3)2∥·C3H6O and ∥RevOX2(C6H7N2S)(PPh3)∥ (X=Cl, Br). The crystal structures oftrans-∥ReCl2(C6H7N2S)(PPh3)2∥·C3H6O (I) and ∥ReOCl2(C6H7N2S)(PPh3)∥ (II) have been determined from single-crystal diffractometer data and refined toR factors of 0.0496 and 0.0365, respectively. (I) crystallizes in the triclinic space group P¯1 witha=16.875(4),b=13.969(7),c=9.510(2) Å;α=81.78(2)°,β=85.15(12)°, γ=107.97(8)° andZ=2. The coordination geometry around the rhenium center exhibit mutuallytrans phosphine groups and chloride ligands disposedtrans to the nitrogen and sulfur donors of the pyrimidinethiolate ligand which form a four-membered chelate ring with the metal. (II) crystallizes in the monoclinic space group P21/c witha=12.554(3),b=10.501(1),c=19.200(5) Å;β=106.54(2)° andZ=4. The rhenium atom presents a very distorted octahedral configuration with a chlorine atomtrans to phosphine ligand in the axial position and the N,S-chelate ligand in the equatorial plane with the sulfur donor atomtrans the Re=Ooxo group. The compounds were characterized also by means of ir and nmr spectroscopic measurements; reaction pathways are discussed on the basis of structural data.

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Authors and Affiliations

  1. Dipartimento di Chimica, University of Modena, Via Campi 183, 41100, Modena, Italy

    R. Battistuzzi & T. Manfredini

  2. Istituto di Chimica Generale ed Inorganica Centra di Studio per la Strutturistica Diffrattometrica del C.N.R., University of Parma, Viale delle Scienze, 43100, Parma, Italy

    L. P. Battaglia & A. Bonamartini Corradi

  3. Dipartimento di Chimica Inorganica, Metallorganica ed Analitica, University of Padova, Via Loredan 4, 35100, Padova, Italy

    A. Marzotto

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  1. R. Battistuzzi
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  4. A. Bonamartini Corradi
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Battistuzzi, R., Manfredini, T., Battaglia, L.P. et al. Synthesis, structural, and spectroscopic study of rhenium(III) and rhenium(V) 4,6-dimethylpyrimidine-2-thiolate/triphenylphosphine mixed complexes: Crystal and molecular structure of ∥ReCl2(pymS)(PPh3)2∥·C3H6O and ∥ReOCl2(pymS)(PPh3)∥. Journal of Crystallographic and Spectroscopic Research 19, 513–534 (1989). https://doi.org/10.1007/BF01185388

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