Synthesis and Structural Characterization of Neutral Silver(I) Complexes with Arenephosphinothiols. Crystal Structures of [Ag4{2-(Ph2P)-6-(Me3Si)C6H6
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- 作者：Paulo Perez-Lourido ; Jose A. Garcia-Vazquez ; Jaime Romero ; Antonio Sousa ; Eric Block ; Kevin P. Maresca ; and Jon Zubieta
- 刊名：Inorganic Chemistry
- 出版年：1999
- 出版时间：February 8, 1999
- 年：1999
- 卷：38
- 期：3
- 页码：538 - 544
- 全文大小：112K
- 年卷期：v.38,no.3(February 8, 1999)
- ISSN：1520-510X
文摘
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 procedureand characterized by spectroscopic (IR, 1H, 13C, and 31P NMR) methods, and ligand 3 and [Ag4{2-(Ph2P)-6-(Me3Si)C6H3S}4] (5) and [Ag4{2-(Ph2PO)-6-(Me3Si)C6H3S}4] (6) complexes were characterized by X-raycrystallographic 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, 
= 103.961(1)
, V = 2107.4(1) Å3, Z = 4, 2730 reflections with Io > 2
(Io),R = 0.0621. Crystal data for 5: C84H88Ag4P4S4Si4, 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 > 2(Io), R = 0.0286. Crystal data for 6:C90H97Ag4N3O4P4S4Si4, trigonal, P1, a = 13.4567(1) Å, b = 14.4148(2) Å, c = 14.8080(2) Å, 
= 99.130(1), = 98.815(1), g = 114.211(1), V = 2509.38(5) Å3, Z = 1, 6345 reflections with Io > 2(Io), R = 0.0505. The[Ag4{2-(Ph2P)-6-(Me3Si)C6H3S}4] (5) compound is tetranuclear with an array of four silver atoms bridged byfour sulfur atoms. Each silver atom has a distorted trigonal [AgS2P] environment with each ligand acting as P,Sbidentate S-bridging ligand. The [Ag4(2-(Ph2PO)-6-(Me3Si)C6H3S}4] (6) complex is also tetranuclear, but in thiscase two of the silver atoms are [AgO2S2] tetracoordinated and the other two Ag atoms are [AgS2] two coordinated.
= 103.961(1), V = 2107.4(1) Å3, Z = 4, 2730 reflections with Io > 2(Io),R = 0.0621. Crystal data for 5: C84H88Ag4P4S4Si4, 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 > 2(Io), R = 0.0286. Crystal data for 6:C90H97Ag4N3O4P4S4Si4, trigonal, P1, a = 13.4567(1) Å, b = 14.4148(2) Å, c = 14.8080(2) Å, = 99.130(1), = 98.815(1), g = 114.211(1), V = 2509.38(5) Å3, Z = 1, 6345 reflections with Io > 2(Io), R = 0.0505. The[Ag4{2-(Ph2P)-6-(Me3Si)C6H3S}4] (5) compound is tetranuclear with an array of four silver atoms bridged byfour sulfur atoms. Each silver atom has a distorted trigonal [AgS2P] environment with each ligand acting as P,Sbidentate S-bridging ligand. The [Ag4(2-(Ph2PO)-6-(Me3Si)C6H3S}4] (6) complex is also tetranuclear, but in thiscase two of the silver atoms are [AgO2S2] tetracoordinated and the other two Ag atoms are [AgS2] two coordinated.