The resolution of CpMo(NO)(methylallyl)(X) complexes. X-ray crystal structures of (−)-CpMo(NO)(syn-crotyl)(1S)-10- camphorsulfonate) and (μ-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 P212121 with dimensions a=7.039(1), b=9.2797(6), c=38.254(5) Å, V=2498.8(6) Å3 and Z=4. A partial kinetic resolution of racemic CpMo(NO)(ν3-2-MeC3H4)I has been carried out by reaction with (R)-(−)-myrtenal in CD2Cl2 and a trace of water, which leaves the (R)-(+)-CpMo(NO)(ν3-2-MeC3H4)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 (μ-OH)2[CpMo(NO)I]2 was formed. It crystallizes in a monoclinic cell with a space group of P21/n with dimensions a=10.457(1), b=15.976(1), c=11.076(1) Å, β=115.989(3)°, V=1663.3(3) Å3 and Z=4.