The complex [Mo(CO)3(η-C5Me5)(PPh3)]BF4(1) reacts with NaN3 in methanol solution to give a mixture of cis-[Mo(CO)2(η-C5Me5)(PPh3)(N3)](2) and cis-[Mo(CO)2(η-C5Me5)(PPh3)(NCO)](3), which were separated as pure products by column chromatography. Pure (3) was also obtained by an independent route, i.e. by treating a methanol solution of (1) with cyanate ion. The solid-state structures of complexes (2) and (3) were determined by single-crystal X-ray diffraction: they are isomorphous, space group P21/c(no. 14); for (2), a= 8.625(2), b= 18.655(9), c= 17.573(5)Å, β= 92.29(2)°, Z= 4,3 315 independent data [Io > 2.5σ(Io)] refined to R= 0.032, R′= 0.034; for (3), a= 8.641 (1), b= 18.547(3), c= 17.52(1)Å, β= 91.15(3)°,Z= 4, 2 045 independent data [Io > 2.5σ(Io)] refined to R= 0.044, R′= 0.046. Differences in the co-ordination geometry of the N3– and NCO– ligands are discussed.
Reactivity of cationic molybdenum(II) complexes. Part 4. Isolation and crystal structure determination of cis-[Mo(CO)2(?-C5Me5)(PPh3)(N3)] and cis-[Mo(CO)2(?-C5Me5)(PPh3)(NCO)]
LEONI, PIERO;PASQUALI, MARCO;
1989-01-01
Abstract
The complex [Mo(CO)3(η-C5Me5)(PPh3)]BF4(1) reacts with NaN3 in methanol solution to give a mixture of cis-[Mo(CO)2(η-C5Me5)(PPh3)(N3)](2) and cis-[Mo(CO)2(η-C5Me5)(PPh3)(NCO)](3), which were separated as pure products by column chromatography. Pure (3) was also obtained by an independent route, i.e. by treating a methanol solution of (1) with cyanate ion. The solid-state structures of complexes (2) and (3) were determined by single-crystal X-ray diffraction: they are isomorphous, space group P21/c(no. 14); for (2), a= 8.625(2), b= 18.655(9), c= 17.573(5)Å, β= 92.29(2)°, Z= 4,3 315 independent data [Io > 2.5σ(Io)] refined to R= 0.032, R′= 0.034; for (3), a= 8.641 (1), b= 18.547(3), c= 17.52(1)Å, β= 91.15(3)°,Z= 4, 2 045 independent data [Io > 2.5σ(Io)] refined to R= 0.044, R′= 0.046. Differences in the co-ordination geometry of the N3– and NCO– ligands are discussed.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
