Peter Maitlis - Academia.edu (original) (raw)
Papers by Peter Maitlis
Inorganica Chimica Acta, 1995
The reactions of complex (CsMe5)Ir(C1)(CO)(Me) (la) with cyclohexylisocyanide and phosphines (L=C... more The reactions of complex (CsMe5)Ir(C1)(CO)(Me) (la) with cyclohexylisocyanide and phosphines (L=CyNC, PHPh2, PMePh2, PMe2Ph) give the products of alkyl migratory insertion (CsMes)Ir(C1)(COMe)(L), in toluene or tetrahydrofuran at 323 K or higher temperature. The phenyl analogue (C5Me5) Ir (C1) (CO) (Ph) or the iodide complexes (C~Mes) Ir (I) (CO) (R) ( R = Me, Ph ) are not reactive under the same conditions. The reaction of (C5Me~) Ir (C1) (CO) (Me) with PMePh2 and PMe2Ph in acetonitrile yields the chloride substitution product [ (CsMes)Ir(CO) (L) (Me) ] +CI-. Kinetic measurements for the reactions of (C~Mes)Ir(C1) (CO) (Me) in toluene are first order in the iridium complex and exhibit a saturation dependence on the incoming donors L. Analysis of the data suggests a two-step process involving (i) rapid formation of a molecular complex [ (C5Mes)Ir(C1) (CO) (Me), (L) ], in which the structure of la is unperturbed within the limits of spectroscopic analysis, and (ii) rate determining methyl migration. The reaction parameters are K for the pre-equilibrium step (K= 1.5 (CyNC), 7.3 (PHPh2), 7.1 (PMePh2) dm 3 mol-1 at 323 K) and k2 for the slow carbon-carbon bond formation (k2(10 s) =6.9 (CyNC), 1.2 (PHPh2), 1.0 (PMePh2) s-1 at 323 K). The activation parameters for the methyl migration step in the reaction with PMePh2, obtained between 308 and 338 K, are AH ~ = 106_+ 16 kJ mol-~ and AS* = -14 + 5 J K-1 mol-1. The reaction of la with PMePh2 proceeds at similar rates in tetrahydrofuran (K = 3.7 dm 3 mol-1, k2 ( 1 05 ) = 1.2 s-1,323 K). The crystal structure of (CsMe 5) lr (C1) (COMe) (PMe2Ph) has been determined by X-ray diffraction. C2oH29CIOPIr: Mr = 544.1, monoclinic, P21/n, a = 8.084(2), b = 9.030(2), c = 28.715(3) /~, fl = 91.41 (3)°, Z = 4, D c = 1.71 g cm-3 V = 2095.5/~3 room temperature, Mo K a, A = 0.71069,/z = 65.55 cm-~, F(000) = 1044, R = 0.037 for 2453 independent observed reflections. The complex shows a deformed tetrahedral coordination assuming the r/5-CsMe5 molecular fragment as a single coordination site. The iridium-chlorine bond is staggered with respect to two adjacent C(ring)-methyl bonds, while the Ir-P and the k-COMe bonds are eclipsed with respect to C (ring)-methyl bonds. * Dedicated to Professor Fred Basolo on his 75th birthday. * Corresponding authors. 0020-1693/95/$09.50 © 1995 Elsevier Science S.A. All rights reserved SSD10020-1693 (95)04573-R We have recently reported a direct rate comparison between rhodium and iridium (M) for the oxidative addition of methyl iodide to [M(CO)212]-and to [(CsMes)M-(CO) 2 ], and for the methyl migratory insertion in [ (C5Me 5)-M(CI) (CO)Me] [3]. The migration of methyl onto CO in corresponding systems is 105-106 times faster for Rh(III) than for Ir(III).
Inorganica Chimica Acta, 1995
The reactions of complex (CsMe5)Ir(C1)(CO)(Me) (la) with cyclohexylisocyanide and phosphines (L=C... more The reactions of complex (CsMe5)Ir(C1)(CO)(Me) (la) with cyclohexylisocyanide and phosphines (L=CyNC, PHPh2, PMePh2, PMe2Ph) give the products of alkyl migratory insertion (CsMes)Ir(C1)(COMe)(L), in toluene or tetrahydrofuran at 323 K or higher temperature. The phenyl analogue (C5Me5) Ir (C1) (CO) (Ph) or the iodide complexes (C~Mes) Ir (I) (CO) (R) ( R = Me, Ph ) are not reactive under the same conditions. The reaction of (C5Me~) Ir (C1) (CO) (Me) with PMePh2 and PMe2Ph in acetonitrile yields the chloride substitution product [ (CsMes)Ir(CO) (L) (Me) ] +CI-. Kinetic measurements for the reactions of (C~Mes)Ir(C1) (CO) (Me) in toluene are first order in the iridium complex and exhibit a saturation dependence on the incoming donors L. Analysis of the data suggests a two-step process involving (i) rapid formation of a molecular complex [ (C5Mes)Ir(C1) (CO) (Me), (L) ], in which the structure of la is unperturbed within the limits of spectroscopic analysis, and (ii) rate determining methyl migration. The reaction parameters are K for the pre-equilibrium step (K= 1.5 (CyNC), 7.3 (PHPh2), 7.1 (PMePh2) dm 3 mol-1 at 323 K) and k2 for the slow carbon-carbon bond formation (k2(10 s) =6.9 (CyNC), 1.2 (PHPh2), 1.0 (PMePh2) s-1 at 323 K). The activation parameters for the methyl migration step in the reaction with PMePh2, obtained between 308 and 338 K, are AH ~ = 106_+ 16 kJ mol-~ and AS* = -14 + 5 J K-1 mol-1. The reaction of la with PMePh2 proceeds at similar rates in tetrahydrofuran (K = 3.7 dm 3 mol-1, k2 ( 1 05 ) = 1.2 s-1,323 K). The crystal structure of (CsMe 5) lr (C1) (COMe) (PMe2Ph) has been determined by X-ray diffraction. C2oH29CIOPIr: Mr = 544.1, monoclinic, P21/n, a = 8.084(2), b = 9.030(2), c = 28.715(3) /~, fl = 91.41 (3)°, Z = 4, D c = 1.71 g cm-3 V = 2095.5/~3 room temperature, Mo K a, A = 0.71069,/z = 65.55 cm-~, F(000) = 1044, R = 0.037 for 2453 independent observed reflections. The complex shows a deformed tetrahedral coordination assuming the r/5-CsMe5 molecular fragment as a single coordination site. The iridium-chlorine bond is staggered with respect to two adjacent C(ring)-methyl bonds, while the Ir-P and the k-COMe bonds are eclipsed with respect to C (ring)-methyl bonds. * Dedicated to Professor Fred Basolo on his 75th birthday. * Corresponding authors. 0020-1693/95/$09.50 © 1995 Elsevier Science S.A. All rights reserved SSD10020-1693 (95)04573-R We have recently reported a direct rate comparison between rhodium and iridium (M) for the oxidative addition of methyl iodide to [M(CO)212]-and to [(CsMes)M-(CO) 2 ], and for the methyl migratory insertion in [ (C5Me 5)-M(CI) (CO)Me] [3]. The migration of methyl onto CO in corresponding systems is 105-106 times faster for Rh(III) than for Ir(III).