The formation and X-ray crystal structure of (η5-C5H5)2LuCl•OC4H8

Abstract LuCl 3 reacts with two equivalents of sodium cyclopentadienide in THF followed by crystallization from this solvent at 5°C to afford (C 5 H 5 ) 2 LuCl · OC 4 H 8 . The product has been characterized by its proton NMR and mass spectra, elemental analysis and by single crystal X-ray diffraction studies. The complex (C 5 H 5 ) 2 LuCl · OC 4 H 8 crystallizes in the monoclinic space group P 2 1 / n with the unit cell parameters, a 8.116(2), b 12.670(2), c 14.376(1) A, β 105.61(1)°, V 1423.7 A 3 , Z = 4, D c 1.925 g cm −3 . The structure was solved by heavy-atom Patterson techniques and the least-squares refinement has led to a final R value of 0.097 based on 2253 independent observed reflections. The THF molecule is coordinated to the lutetium atom at a LuO bond length of 2.27(1) A. The LuC(η5) bond distances average 2.56 A. The compound (η 5 -C 5 H 5 ) 2 LuCl · OC 4 H 8 is a neutral monomer.