Abstract
The reaction of the Re(III) complex [ReCl 3(NNC 5H 4NH) (HNNC 5H 4N)] ( 1) with triphenylphosphine and a proton scavenger in methanol gives the neutral complex [ReCl 2(PPh 3) (NNC 5H 4N) (HNNC 5H 4N)] ( 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(PPh 3) (NNHC 5H 4N) (HNNC 5H 4N)] + 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 ReCl 2PN 6C 28H 26: monoclinic space group P2 I/ n, a = 10.263(2), b = 14.938(3), c = 19.650(4) A ̊ , β = 97.54(3)° with Z = 4 to give V = 2995.5(15) A ̊ 3 . The coordination geometry is distorted octahedral. The ReN bond length to the pyridine nitrogen atom of the organodiazene chelate is 2.147(15) Å, while the ReN bond to the diazene-α-nitrogen atom is 1.915(21) Å. The NN bond length of this ligand is 1.340(26) Å, indicative of multiple bonding within the chelated ligand. The ReN bond length of the pyridyldiazenido ligand is 1.778(14) Å, and the NN bond length is 1.212(22) Å, again reflecting the multiple bonding throughout the singly-bent, organodiazenido unit. The bond angle of the ReNN linkage is 172.8(13)°.
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