THE RESOLUTION OF CPMO(NO) (METHYLALLYL)(X) COMPLEXES - X-RAY CRYSTAL-STRUCTURES OF (-)-CPMO(NO)(SYN-CROTYL)((1S)-10-CAMPHORSULFONATE) AND (MU-OH)(2)[CPMO(NO)I](2)

The 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 MoCl3SO5NC20H28, and in an orthorhombic cell with a space group of P2(1)2(1)2(1) with dimensions a=7.039(1), b=9.2797(6), c=38.254(5) Angstrom, V=2498.8(6) Angstrom(3) and Z=4. A partial kinetic resolution of racemic CpMo(NO)(eta(3)-2-MeC(3)H(4))I has been carried out by reaction with (R)-(-)-myrtenal in CD2(C)l(2) and a trace of water, which leaves the (R)-(+)-CpMo(NO)(eta(3)-2-MeC(3)H(4))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 (mu-OH)(2)[CpMo(NO)I](2) was formed. It crystallizes in a monoclinic cell with a space group of P2(1)/n with dimensions a=10.457(1), b=15.976(1), c=11.076(1) Angstrom, beta=115.989(3)degrees V=1663.3(3) Angstrom(3) and Z=4.