Abstract
The reaction of [TeCl 3(NNC 5H 4NH)(HNNC 5H 4N)] with thiophenol and trialkylamine in methanol gives [Tc(SPh) 2(NNC 5H 4N)(HNNC 5H 4N)] 2 in excellent yields. The neutral, paramagnetic, doubly thiolato-bridged dimer contains a pyridyldiazenido ligand and a bidentate organodiazene ligand on each of the technetium atoms, as well as a terminal and a bridging phenyl-thiolate ligand. The infrared spectrum displays a series of strong absorption in the 1600-1150 cm 1 region from the two organohydrazide ligands. The fast atom bombardment (+) mass spectrum displays the protonated parent ion {[Te 2(SPh) 4(NNC 5H 4N) 2(HNNC 5H 4N) 2]·H} + of 1061 m/ z and the fragment [Te 2(SPh) 3(NNC 5H 4N) 2(HNNC 5H 4N) 2] + of 951 m/ z. The X-ray structure displays a molecular coordination geometry of distorted octahedral. The TeN bonnd length to the pyridine nitrogen atom of the organodiazene chelate is 2.135(8) A, while the TeN bond to the diazene α-nitrogen atom is 2.016(8) A. The NN bond length of this ligand is 1.285(11) A, indicative of multiple bonding within the chelated ligand. The TeN bond length of the pyridyldiazenido ligand is 1.778(10) A and the NN bond length is 1.237(11) A, again reflecting the multiple bonding throughout the organodiazenido unit. The bond angle for this linkage is 174.2(8)″. Crystal data for TeS 2N 6C 22H 19; orthorhombic space group Pbca; unit cell dimensions: a = 15.176(3), b = 16.560(5), c = 19.875(5) A ̊ V = 4995(2) A ̊ , with D = 1.408 g cm 1 to give Z = 8. Structure solution based on 2325 reflections converged at R = 0.0753 for ( I · 2 σ( I)).
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