Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh3)2(NHNC5H4N)(HNNC 5H4N)]Cl2, [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}]

Paulo Pérez-Lourido, Jaime Romero, J. A. García-Vázquez, Antonio Sousa, Kevin P. Maresca, Jon Zubieta

Research output: Contribution to journalArticle

12 Scopus citations

Abstract

The reduction of ReO4- with 2-hydrazinopyridine dihydrochloride and PPh3 gives [ReCl(PPh3)2(NHNC5H4N)-(HNNC 5H4N)]Cl2 (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh3 in methanol hydrochloric acid allows the preparation of [ReCl3(PPh3)2(NNC3H 4N2)] (3). The reaction of the Re(III) complex [ReCl3(NNC5H4-NH)(HNNC5H 4N)] (1), with 2-(Ph2P)C6H4SH in methanol yields [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}-(NNC5H4N)(HNNC 5H4N)] (4) and [Re{2-(Ph2P)C6H4S}2(NNC 5H4N)] (5). The same precursor with 2-(Ph2PO)-6-(Me3Si)C6H3SH gives [ReCl{2-(Ph2PO)-6-(Me3Si)C6H 3S}(NNC5H4N)(HNNC5H4N)] (6) and with PhP(C6H4SH-2)2 yields [Re{PhP(C6H4S-2)2}(NNC5H 4N)(HNNC5H4N)] (7). Crystal data: 2, C46H39N6P2Cl3Re, orthorhombic, Pnma, a = 19.6381(7) Å, b = 15.1861(6) Å, c = 15.0711(5) Å, V = 4494.6(3) Å3, Z = 6, 5646 reflections, R = 0.0655; 4, C46H37N6OP2S2Re, triclinic, P1̄, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, α = 61.88(10)°, β= 80.9220(10)°, γ = 85.1350(10)°, V = 2124.40(7) Å3, Z = 2, 8728 reflections, R = 0.0757; 5, monoclinic, P21/c, a = 10.0006(2) Å,b= 18.1857(1) Å, c = 19.8595(2) Å, β= 94.09(1)°, V= 3598.08(8) Å3, Z = 4, 8406 reflections, R = 0.0359.

Original languageEnglish (US)
Pages (from-to)1511-1519
Number of pages9
JournalInorganic Chemistry
Volume38
Issue number7
StatePublished - Dec 1 1999

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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