The resolution of CpMo(NO)(methylallyl)(X) complexes. X-ray crystal structures of (−)-CpMo(NO)(syn-crotyl)(1S)-10- camphorsulfonate) and (ì-OH)2[CpMo(NO)I]2.

J.W. FALLER ; K.J. CHASE; M.R. MAZZIERI

ELSEVIER SCIENCE SA

Lugar: Amsterdam; Año: 1995 vol. 229 p. 39 - 39

he resolution of the chiral metal center in CpMo(NO)(syn-crotyl)((1S)-10-camphorsulfonate) has been effected by fractional crystallization. An X-ray crystal structure determination of the (-)-diastereomer reveals an (S) configuration at the metal. It crystallizes from chloroform as a solvate having a formula of MoCI3SOsNCa0H2s and in an orthorhombic cell with a space group of P212~21 with dimensions a=7.039(1), b=9.2797(6), c=38.254(5) /~,, V=2498.8(6) /~3 and Z-4. A partial kinetic resolution of racemic CpMo(NO)(rt3-2-MeC3I-I4)I has been carried out by reaction with (R)-(-)-myrtenal in CD2C12 and a trace of water, which leaves the (R)-(+)-CpMo(NO)(@-2-MeC3I-I4)I isomer in 45% enantiomeric excess after 77% conversion of the starting material. In addition to the organic product, an insoluble crystalline material identified by X-ray crystallography as (~-OH)2[CpMo(NO)I]2 was formed. It crystallizes in a monoclinic cell with a space group of P2Jn with dimensions a=10.457(1), b=15.976(1),