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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 14, Number 2
BKCSDE 14(2)
February 20, 1993 

Synthesis of Alkylidyne Complexes of Br(CO)2(tmeda)M≡CC6H4Me (M = Cr, Mo, W). Crystal Structure of Br(CO)2(tmeda)Cr≡CC6H4Me
Joon T. Park*, Jeong-Ju Cho, Il-Hwan Suh, Jin-Ho Lee, Sung-Su Lim, Bo-Young Ryu
The reaction of (CO5)M=C(OMe)Tol (M=Cr, Mo, W and Tol=p-C6H4Me) and BBr3 followed by treatment with tetramethylethylenediamine (TMEDA) yields a mixture of two diastereomers, trans, cis-Br(CO)2(tmeda)M≡CTol [M=Cr(1a), Mo(2a), W(3a)] and cis, trans-Br(CO)2(tmeda)M≡CTol [M=Cr(1b), Mo(2b), W(3b)], respectively. These compounds have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, 1H and 13C-NMR) data. The trans, cis-Br(CO)2(tmeda)Cr≡CTol (1a), has been examine via a single crystal X-ray diffraction study : BrCrO2N2C16H23, Mr=407.27, triclinic, P1, a= 12.792(2), b= 13.400(5), c= 11.645(4) Å, α= 101.26(2)°, β= 103.04(2)°, γ= 91.88(2)°, V= 1907(l) Å3, Z= 2, ρ(calcd)= 1.418 gcm-3, λ (MoKα)= O.71069 Å, μ= 26.25 cm-1, F(000)= 831.97, T= 295 K, R= 0.0977 for 1332 significant reflections [F0>5σ(F0)]. There are two essentially equivalent molecules in the crystallographic asymmetric unit. Each molecule is octahedral with the bromide ligand trans to the alkylidyne carbon, the two cis-carbonyl ligands, and the bidentate TMEDA ligand.
266 - 271
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