Journal of Organometallic Chemistry p. 121 - 127 (1998)
Update date:2022-08-03
Topics:
Borwieck
Walter
Dinjus
Rebizant
Cyclotrimerization of t-butylacetylene or phenylacetylene with CpCo(CO)2 as catalyst in supercritical water yields the isomeric 1,3,5-tris-substituted- (1: R=Ph, 1a: R=but) and 1,2,4-tris-substituted benzene derivatives (2: R=Ph, 2a: R=but). The identification of the organometallic products obtained under these conditions is described. The formation of all possible isomers of the corresponding CpCo(bis-substituted-cyclobutadiene) (3, 4), CpCo(bis-substituted-CpCobaltacyclopentadiene) (5, 6, 7) and CpCo(bis-substituted-cyclopentadienone) (8, 9, 10) via GC-MS is reported. Two of three isomers of CpCo(bis-substituted-cyclopentadienone) (8, 9 (R=Ph), 8a, 9a (R=but)) were separated and characterized in substance. The structures of 8, 9, 8a and 9a were elucidated by single crystal X-ray diffraction. 8 crystallizes in the orthorhombic space group P212121 (No.19) with a=840.5(1), b=1105.9(2), c=1767.2(3) pm, V=1642.8(1)×106 pm3, Z=4, Dcalc=1.441 g cm-3, R1=0.0501 (I>3σ), wR1=0.0529 (I>3σ). 9 crystallizes in the orthorhombic space group Pna21 (No.33) with a=1086.7(1), b=4726.0(1), c=1668.5(1) pm, V=8427.3(1)×106 pm3, Z=20, Dcalc=1.404 g cm-3, R1=0.0705 (I>2σ), Rw=0.1321 (all data on F2). 8a crystallizes in the monoclinic space group P21/c (No. 14) with a=1441.6(3), b=1241.3(1), c=3672.6(6) pm, β=92.39(2)°, V=6566(2)×106 pm3, Z=16, Dcalc=1.280 g cm-3, R1=0.082 (I>2σ), Rw=0.144 (all data on F2). 9a crystallizes in the monoclinic space group P21/c (No. 14) with a=669.3(1), b=1335.7(1), c=1843.1(1) pm,β=94.78(1)°, V=1641.9(1)×106 pm3, Z=4, Dcalc=1.28 g cm-3, R1=0.0622 (I>2σ), Rw=0.1185 (all data on F2).
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