Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2], ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}

Paulo Perez-Lourido, J. Romero, J. Garcia-Vazquez, Antonio Sousa, Kevin P. Maresca, David J. Rose, Jon Zubieta

Research output: Contribution to journalArticle

28 Scopus citations

Abstract

The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC6H4)P(C6H4X)2, where X = H or SH [abbreviated P-(SH),x (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the {M(P-Sx)2} core, represented by [Re{P(C6H4S)3}{P(C6H 4S)2(C6H4SH)}] (1), [ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}] (3), and [ReOCl{OP(C6H5)2(2-SC6H 3-3-SiMe3)}2] (5). The reaction of 1 with NEt3 results in the formation of [HNEt3][Re{P(C6H4S)3}2] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl{OP- (C6H5)2(2-SC6H 3-3-SiMe3)}2] (4). Crystal data: 2, C43H42NP2S6Cl2Re, monoclinic, P21/c, a = 14.2484(2) Å, b = 15.3108(1) Å, c = 19.5121(2) Å, β= 90.366(1)°, V = 4256.56(8) Å3, Z = 2, 26 410 reflections, R = 0.0605; 3, C36H28O2P2S 2ClRe,triclinic, P1̄, a = 9.3427(1) Å, b = 11.9075(1) Å, c = 16.8504(1) Å, α = 98.177(1)°, β= 104.132(1)°, y = 109.000(1)°, V = 1667.79(2) Å3, Z = 2, 7567 reflections, R = 0.0333; 4, C36H28O5P2S2Re 2, monoclinic, P21/n, a = 10.6714(1) Å, b = 24.0076(2) Å, c = 13.3610(1) Å, β= 93.65(1)°, V = 3416.51(4) Å3, Z = 4, 8073 reflections, R = 0.0469; 5, C44H47NO3Si2P2S 2ClRe, triclinic, P1̄, a = 10.1616(2) Å, b = 14.7095(3) Å, c = 17.0744(3) Å, α = 89.108(1)°, β= 83.634(1)°, γ = 70.901(1)°, V = 2396.21(8) Å3, Z = 2, 6175 reflections, R = 0.0837.

Original languageEnglish (US)
Pages (from-to)3331-3336
Number of pages6
JournalInorganic Chemistry
Volume37
Issue number13
DOIs
StatePublished - 1998

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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