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).
The molecular structure of [Mo(CO)3H(-C5Me5)] and its conversion to [Mo(CO)3Cl(-C5Me5)] and [Li(Me2NCH2CH2NMe2)2][Mo(CO)3(-C5Me5)]
LEONI, PIERO;PASQUALI, MARCO;
1986-01-01
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).I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
