186379-82-8Relevant academic research and scientific papers
Synthesis and characterization of ring-coupled cyclopentadienyl and indenyl bimetallic derivatives of Cr, Mo and W
Fierro, Ricardo,Bitterwolf, Thomas E.,Rheingold, Arnold L.,Yap, Glenn P. A.,Liable-Sands, Louise M.
, p. 19 - 30 (1996)
A series of new ring-coupled bimetallic complexes M2(CO)6[η5,η5-C5H4-C(CH3)2-C5H4], where M = Cr, Mo, W, was synthesized by reaction of the dianion of the ligand 2,2-bis(cyclopentadienyl)propane and M(CO)3(CH3CN)3, M = Cr, Mo, W. Oxidation with acetic acid-Fe(III) produced the bimetallic complexes in moderate yields. Using the same strategy, reactions of Mo(CO)3(CH3CN)3 with the dianion of 2-cyclopentadienyl-2-indenylpropane produced only the dimer [Mo(CO)3[η5-C5H4-C(CH3)2-C9H7]2 in which the indenyl ring was unmetallated. Subsequent detailed studies revealed that the desired dimetalloanion was initially formed, but that the indenyl bound metal was lost upon protonation. Evidence for the mechanism of this demetallation process is presented. The dimetalloanion could be intercepted by methyl iodide to form [Mo(CO)3CH3]2[η5,η5-C5H4-C(CH3)2-(C9H6)]. Synthesis of Mo2(CO)6[η5,η5-C5H4-C(CH3)2-(3-RC9H5)], where R = H, CH3, was achieved by aprotic oxidation of the intermediate dimetalloanion by ferricinium tetraphenylborate. The molecular structures of two compounds are reported: Mo2(CO)6[η5,η5-C5H4-C(CH3)2-(3-CH3C9H5)]: triclinic, P1, a = 8.777(3) A, b = 9.428(4) A, c = 14.915(4) A, α = 91.42(3)°, β = 102.04(3)°, γ=114.69(3)°, V-1087.9(8) A3, Z = 2, R(F) = 3.03%.[Mo(CO)3CH3]2[η5,η5-C5H4-C(CH3)2-(C9H6)]: triclinic, P1, a = 8.298(6) A, b= 11.662(6) A, c= 13.241(8) A, a = 100.28(1)°, β = 93.02(l)°, γ - 99.72(1)°, V-1238(1) A3, Z=2, R(F) = 3.99.%.
