The molecular structure of [Mo(CO)3H(η-C5Me5)] and its conversion to [Mo(CO)3Cl(η-C5Me5)] and [Li(Me2NCH2CH2NMe2)2][Mo(CO)3(η-C5Me5)]

Abstract

Crystals of [Mo(CO)₃H(η-C₅Me₅)](1) suitable for an X-ray structural determination were obtained by reacting equimolar amounts of [Mo(CO)₃(C₇H₈)](C₇H₈= cycloheptatriene) and C₅HMe₅ in methanol under hydrogen at room temperature. Complex (1) crystallizes in the monoclinic space group P2₁ in a unit cell of dimensions a= 8.003(2), b= 12.874(3), c= 7.087(2)Å, β= 103.06(2)°, and Z= 2; R′= 0.047 for 1 136 observed reflections. Complex (1) reacts at room temperature with CCl₄ to give [Mo(CO)₃Cl(η-C₅Me₅)](2), and with LiBuⁿ in the presence of tetramethylethylenediamine (tmen) to give [Li(tmen)₂][Mo(CO)₃(η-C₅Me₅)](3). Complexes (2) and (3) were isolated in high yields and were analytically and spectroscopically characterized. Complex (1) does not react with CO₂(1 atm), CO₂(1 atm), or with other CO₂-like molecules (CS₂, p-tolylcarbodi-imide).