New cyclic tellurides. Synthesis, reaction and ligand properties of 2,2,6,6-tetramethyl-1-oxa-4-tellura-2,6-disilacyclohexane (C6H16OSi2Te). X-Ray structure determination of C6H16OSi2TeI2 |
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Authors: | Ali Z. Al-Rubaie Sakae Uemura Hideki Masuda |
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Affiliation: | Department of Chemistry, University of Basrah, Basrah Iraq Institute for Chemical Research, Kyoto University, Uji, Kyoto 611 Japan Coordination Chemistry Laboratories, Institute for Molecular Science, Myodaiji, Okazaki 444 Japan |
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Abstract: | A new tellurium-containing heterocyclic compound, 2,2,6,6-tetramethyl-1-oxa-4-tellura-2,6-disilacyclohexane (C6H16OSi2Te) (1), has been prepared by treatment of 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane with sodium telluride. Mononuclear and dinuclear palladium complexes of this telluride have been prepared by the reaction of 1 with PdCl2(PhCN)2 and Na2PdCl4, respectively. The following new derivatives of 1 have also been produced: C6H16OSi2TeI2 (2), C6H16OSi2TeBr2, C6H16OSi2TeCl2, C6H16OSi2Te(CH3)I, and C6H16OSi2Te(CH2Ph)Br. IR, 1H and 13C NMR and mass spectral data of these new compounds are reported and discussed. 1H NMR studies revealed that in CDCl3 solution both telluronium salts reductively eliminate alkyl halide. The crystal structure of compound 2 has been determined by X-ray diffraction. The compound crystallizes in the monoclinic space group, P21/c, with four molecules in a unit cell of dimension a 12.960(3), b 8.846(2), c 13.754(4) Å, β 92.44(2)°, R = 0.049, and Rw = 0.067 for 3599 unique reflections with |F0| > 3σ(F0). The compound forms a six-membered ring of a slightly displaced boat type. The geometry about the Te atom is pseudo-octahedral, with two carbon atoms (Te-C = 2.156(7) and 2.137(6) Å) and two iodine atoms of the neighbouring molecules (weak intermolecular bonds, Te · I = 3.769 and 3.806 Å) in the equatorial positions and two iodine atoms (Te-I = 2.909(1) and 2.913(1) Å) in the axial positions. |
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