TY - JOUR
T1 - The synthesis, characterization and X-ray crystal structure of the rhenium organodiazenido, organodiazene complex [ReCl2(PPh3)(N=NC5H4N)(HN=NC 5H4N)]
AU - Nicholson, T.
AU - Cook, J.
AU - Davison, A.
AU - Rose, D. J.
AU - Maresca, K. P.
AU - Zubieta, J. A.
AU - Jones, A. G.
N1 - Funding Information:
We thank L. Li of the MIT spectroscopy laboratory for the mass spectrometry results. We also are indebted to the NIH for funding support.
Copyright:
Copyright 2020 Elsevier B.V., All rights reserved.
PY - 1996/11/1
Y1 - 1996/11/1
N2 - 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)°.
AB - 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)°.
KW - Crystal structures
KW - Organodiazene complexes
KW - Organodiazenido complexes
KW - Rhenium complexes
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U2 - 10.1016/s0020-1693(96)05310-8
DO - 10.1016/s0020-1693(96)05310-8
M3 - Article
AN - SCOPUS:0001436564
SN - 0020-1693
VL - 252
SP - 427
EP - 430
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
IS - 1-2
ER -