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Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu 4 ][ReO(H 2 O)Br 4 )]·2H 2 O, [Bu 4 N][ReOBr 4 (OPPh 3 )], [ReO(SC 5 H 4 N) 3 ], [ReO(SC 4 H 3 N 2 ) 3 ][ReO(OH)(SC 5 H 4 N-3,6-(SiMe 2 Bu t ) 2 ) 2 ], [Re(N 2 COC 6 H 5 )(SC 5 H<…

1996; American Chemical Society; Volume: 35; Issue: 12 Linguagem: Estoniano

10.1021/ic950881o

1520-510X

David J. Rose, Kevin P. Maresca, Peter B. Kettler, Yuan Da Chang, Victoria Soghomomian, Qin Chen, Michael J. Abrams, Scott K. Larsen, Jon Zubieta,

Metal complexes synthesis and properties

The syntheses and characterizations of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (1) and its derivatives 3-(trimethylsilyl)pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu4N][ReOBr4(H2O)]·2H2O (5), [Bu4N][ReOBr4(OPPh3)] (6), [ReO2(C5H5N)4], and [Re{N2CO(C6H5)}Cl2(PPh3)2] to give [ReO(C5H4NS)3] (7), [ReO(C8H12NSiS)3] (8), [ReO(OH)(C11H20NSi2S)2] (9), [Re{N2CO(C6H5)}Cl(PPh3)2(C5H4NS)] (10), [ReO(C4H3N2S)3] (11), and [Re{P(C6H5)3}(C4H3N2S)3] (12). Crystal data: 5, C16H42NO4Br4Re, tetragonal, I4̄, a = 8.779(2) Å, b = 11.614(2) Å, c = 9.397(2) Å, β = 114.67(3)°, V = 870.7(4) Å3, Z = 2, 422 reflections, R = 0.0457; 6, C34H51NO2PBr4Re, triclinic, P1̄, a = 14.437(3) Å, b = 16.589(3) Å, c = 16.783(3) Å, α = 94.87(3)°, β = 97.62(3)°, γ = 93.80(3)°, V = 3957(2) Å3, Z = 4, 6141 reflections, R = 0.0758; 7, C15H12N3OS3Re, monoclinic, P21/c, a = 11.533(2) Å, b = 11.385(2) Å, c = 14.039(3) Å, β = 107.97(3)°, V = 1749.8(9) Å3, Z = 4, 1869 reflections, R = 0.0322; 9, C34H65N2O2S2Si4Re, triclinic, P1̄, a = 8.072(2) Å, b = 11.409(2) Å, c = 12.402(3) Å, α = 79.67(3)°, β = 74.05(3)°, γ = 86.18(3)°, V = 1080.2(5) Å3, Z = 1, 4630 reflections, R = 0.0525; 10, C48H39N3OSP2ClRe, triclinic, P1̄, a = 10.842(2) Å, b = 13.660 (3) Å, c = 17.665(4) Å, α = 86.37(3)°, β = 89.93(3)°, γ = 77.22(3)°, V = 2080.2(10) Å3, Z = 2, 4329 reflections, R = 0.0437; 11, C12H9N6OS3Re, orthorhombic, Pbca, a = 8.240(2) Å, b = 13.373(3) Å, c = 29.388(6) Å, V = 3238.4(16) Å3, Z = 8, 1400 reflections, R = 0.0512; 12, C31H26N6S3PCl2Re, triclinic, P1̄, a = 9.224(2) Å, b = 12.050(2) Å, c = 17.665(4) Å, α = 89.25(3)°, β = 85.70(3)°, γ = 67.94(3)°, V = 1604.0(8) Å3, Z = 2, 3592 reflections, R = 0.0697.