The synthesis, characterization and X-ray crystal structure of the rhenium organodiazenido, organodiazene complex [ReCl2(PPh3)(N=NC5H4N)(HN=NC 5H4N)]

T. Nicholson, J. Cook, A. Davison, D. J. Rose, K. P. Maresca, J. A. Zubieta, A. G. Jones

Research output: Contribution to journalArticle

27 Scopus citations

Abstract

The reaction of the Re(III) complex [ReCl3(N=NC5H4NH)(HN=NC5H 4N)] (1) with triphenylphosphine and a proton scavenger in methanol gives the neutral complex [ReCl2(PPh3)(N=NC5H4N)(HN=NC 5H4N)] (2). The neutral, six-coordinate complex contains a singly-bent pyridyldiazenido ligand and a bidentate, organodiazene ligand that is chelated through the pyridine nitrogen atom. The IR spectrum displays a series of strong absorptions in the 1600-1150 cm-1 region characteristic of the organohydrazide ligands. The FAB(+) mass spectrum displays the protonated parent ion of 733 m/z and the ion [ReCl(PPh3) (N=NHC5H4N)(HN=NC5H4N)]+ of 697 m/z. The X-ray crystal structure of this complex displays a cis arrangement of chloride ligands with the pyridine nitrogen atom of the organodiazene chelate located in the position trans to the pyridyldiazenido ligand. Crystal data for ReCl2PN6C28H26: monoclinic space group P21/n, a=10.263(2), b=14.938(3), c=19.650(4) Å, β=97.54(3)° with Z=4 to give V=2995.5(15) Å3. The coordination geometry is distorted octahedral. The Re-N bond length to the pyridine nitrogen atom of the organodiazene chelate is 2.147(15) Å, while the Re-N bond to the diazene-α-nitrogen atom is 1.915(21) Å. The N-N bond length of this ligand is 1.340(26) Å, indicative of multiple bonding within the chelated ligand. The Re-N bond length of the pyridyldiazenido ligand is 1.778(14) Å, and the N-N bond length is 1.212(22) Å, again reflecting the multiple bonding throughout the singly-bent, organodiazenido unit. The bond angle of the Re-N-N linkage is 172.8(13)°.

Original languageEnglish (US)
Pages (from-to)427-430
Number of pages4
JournalInorganica Chimica Acta
Volume252
Issue number1-2
DOIs
StatePublished - Nov 1 1996

Keywords

  • Crystal structures
  • Organodiazene complexes
  • Organodiazenido complexes
  • Rhenium complexes

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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