Synthesis and structural characterization of neutral silver(I) complexes with arenephosphinothiols. Crystal structures of [Ag4{2-(Ph2P)-6-(Me3Si)C6H 6S}4] and [Ag4{2-(Ph2PO)-6-(Me3Si)C6H 3S}4]

Paulo Perez-Lourido, Jose A. Garcia-Vazquez, Jaime Romero, Antonio Sousa, Eric Block, Kevin P. Maresca, Jon Zubieta

Research output: Contribution to journalArticle

28 Scopus citations

Abstract

Silver complexes of the anionic forms of 2-(diphenylphosphino)benzenethiol [2-(PH2P)C6H4SH] (1), 2-(diphenylphosphino)-6-(trimethylsilyl)benzenethiol [2-(Ph2P)-6-(Me3Si)C6H3SH] (2), and 2-(diphenylphosphinyl)-6-(trimethylsilyl)benzenethiol [2-(Ph2PO)-6-(Me3Si)C6H3SH] (3) have been prepared by an electrochemical procedure and characterized by spectroscopic (IR, 1H, 13C, and 31P NMR) methods, and ligand 3 and [Ag4{2-(Ph2P)-6-(Me3Si)C6H 3S}4] (5) and [Ag4{2-(Ph2PO)-6-(Me3Si)C6H 3S}4] (6) complexes were characterized by X-ray crystallographic techniques. Crystal data for 3: C21H23OPSSi, monoclinic, P2(1)/n, a = 11.3730(4) Å, b = 11.1562(4) Å,c= 17.1153(6) Å, β = 103.961(1)°, V = 2107.4(1) Å3, Z = 4, 2730 reflections with Io > 2σ(Io), R = 0.0621. Crystal data for 5: C84H88Ag4P4S4Si 4, tetragonal, P4(2)2(1)2, a = 18.8454(7) Å, b= 18.8454(7) Å, c = 24.596(2) Å, V = 8735.1(7) Å3, Z = 4, 4676 reflections with Io > 2σ(Io), R = 0.0286. Crystal data for 6: C90H97Ag4N3O4P 4S4Si4, trigonal, P1, a = 13.4567(1) Å, b= 14.4148(2) Å, c = 14.8080(2) Å, a = 99.130(1)°, β = 98.815(1)°, g = 114.211(1)°, V = 2509.38(5) Å3, Z = 1, 6345 reflections with Io > 2σ(Io), R = 0.0505. The [Ag4{2-(Ph2P)-6-(Me3Si)C6H 3S}4] (5) compound is tetranuclear with an array of four silver atoms bridged by four sulfur atoms. Each silver atom has a distorted trigonal [AgS2P] environment with each ligand acting as P,S bidentate S-bridging ligand. The [Ag4(2-(Ph2PO)-6-(Me3Si)C6H 3S}4] (6) complex is also tetranuclear, but in this case two of the silver atoms are [AgO2S2] tetracoordinated and the other two Ag atoms are [AgS2] two coordinated.

Original languageEnglish (US)
Pages (from-to)538-544
Number of pages7
JournalInorganic Chemistry
Volume38
Issue number3
StatePublished - Dec 1 1999

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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