SYNTHESIS AND EXPANSION REACTION OF FERROCENYLACETYLENE DIMETAL CARBONYL-COMPOUNDS - THE MOLECULAR-STRUCTURES OF MU-FCCCHCOMO(CO)(5)CP AND MU(3)-FCCHCFECO(2)(CO)(9)

Two ferrocenylacetylene dimetal carbonyl clusters mu-FcCCHCo(CO)(3)M(C O)(2)Cp (2, M = Mo; 3, M = W) were obtained from the reactions of the precursor mu-FcCCHCo(2)(CO)(6) 1 with metal exchange reagents NaM(CO)( 3)Cp in THF under reflux. The dimetal compounds 1, 2, and 3 can furthe r react with Fe-2(CO)(9) in the presence of benzylideneacetone (BDA) t o give the corresponding mu(3)-ferrocenylvinylidene bridged trimetal c lusters mu(3)-FcCHCFeCo(2)(CO)(9) 4 and mu 3-FcCHCFeCoM(CO)(8)Cp (5, M = Mo; 6, M = W), respectively, probably through the formation of the intermediate (BDA)Fe(CO)(3) which acts as an Fe(CO)(3) transfer-reagen t. The new compounds 2-6 were characterized by C/H analysis, IR and H- 1-NMR spectrocopies. The molecular structures of 2 and 4 were determin ed by X-ray structural analysis. 2 is triclinic with space group P (1) over bar (# 2), a = 8.733(2) Angstrom, b = 14.870(3) Angstrom, c = 8. 200(2) Angstrom alpha = 92.77(2)degrees, beta = 101.78(2)degrees, gamm a = 78.41(2)degrees, V = 1021.2(4) Angstrom(3), and Z = 2; final R = 0 .025, R-w = 0.034 for 2988 reflections. Cluster 4 is orthorhombic with space group P2(1)2(1)2(1) (# 19), a = 12.186(5) Angstrom, b = 14.870( 5) Angstrom, c = 7.800(6) Angstrom, V= 2340(2) Angstrom(3) and Z = 4; final R = 0.062, R-w = 0.065 for 2401 reflections. (C) 1998 Elsevier S cience S.A. All rights reserved.