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The reaction of ReOCl 3 (PPh 3 ) 2  and Re 2 O 3 Cl 4 py 4  with (Me 3 Si) 2 NMe yields Re(NMe)Cl 3 (PPh 3 ) 2  ( 1 ) and ReO(OSiMe 3 )Cl 2 py 2  ( 2 ). Re(NMe)Cl 3 (PPh 3 ) 2  crystallizes as  1 ·0.5C 7 H 8  in the monoclinic space group  P 2 1 / c  with  a  = 2556.3(5),  b  = 922.8(4),  c  = 1642.7(7) pm,  β  = 106.21(2)°,  Z  = 4. In the mononuclear complex the Re(V) atom is octahedrally coordinated by three Cl atoms in meridional and two phosphane ligands in trans configuration as well as by one methyl imido group. The methyl imido ligand forms a Re ≡ N triple bond and an almost linear Re ≡ N – Me arrangement with Re – N = 172.2(4) pm and Re – N – Cl = 169.3(5)°.  2  forms monoclinic crystals with the space group  P 2 1 / n  and  a  = 911.0(3),  b  = 1346.3(3),  c  = 1500.5(4) pm,  β  = 95.47(3)°,  Z  = 4. In the octahedral complex the two Cl atoms and the two pyridine ligands are in trans arrangement. The distance Re – O1 = 167.9(3) pm to the terminal oxo ligand and the distance Re – O2 = 188.9(4) pm to the trimethylsiloxy group both represent multiple bonds.

Reaction of heptamethyldisilazane with oxo ligands. Crystal structure of Re(NMe)Cl 3 (PPh 3 ) 2 · 0.5 C 7 H 8 and ReO(OSiMe 3 )Cl 2 py 2