Desulfurization of bibenzyl trisulfide by [CpMo(CO)3]2: Formation and isolation of thiolato-bridged dimolybdenum complexes of [CpMo(CO)2(SBz)]2, [CpMo(CO)(SBz)]2S and [CpMo(SBz)S]2 (Cp=(η5-C5H5), Bz=PhCH2–). Crystal structures of two polymorphs of [CpMo(SBz)S]2
摘要:
The reaction of [CpMo(CO)(3)](2) (1) with a molar equivalent of Bz(2)S(3) at 60 degrees C for 3.5 h has led to the isolation of [CpMo(CO)(2)(SBz)](2) (2), [CpMo(CO)(SBz)](2)S (3) and [CpMo(SBz)S](2) (4) in 16.9%, 3.1% and 61.1% yields, respectively, as main products. Thermolytic studies showed that 2 underwent stepwise decarbonylation to give 3 and 4. All the three products of 2, 3 and 4 were thiolato-bridged dimolybdenum complexes with bond orders of zero, one and two for 2, 3 and 4, respectively. In addition, both 3 and 4 have one and two S atoms bridged in a mu-eta(2)-mode, respectively. The structures of 2 and 3 have been reported previously. The totally decarbonylated 4 was isolated as polymorphs, 4a and 4b, which have been characterized by elemental, spectral analyses and structurally determined. (c) 2007 Elsevier B.V. All rights reserved.
Desulfurization of bibenzyl trisulfide by [CpMo(CO)3]2: Formation and isolation of thiolato-bridged dimolybdenum complexes of [CpMo(CO)2(SBz)]2, [CpMo(CO)(SBz)]2S and [CpMo(SBz)S]2 (Cp=(η5-C5H5), Bz=PhCH2–). Crystal structures of two polymorphs of [CpMo(SBz)S]2
摘要:
The reaction of [CpMo(CO)(3)](2) (1) with a molar equivalent of Bz(2)S(3) at 60 degrees C for 3.5 h has led to the isolation of [CpMo(CO)(2)(SBz)](2) (2), [CpMo(CO)(SBz)](2)S (3) and [CpMo(SBz)S](2) (4) in 16.9%, 3.1% and 61.1% yields, respectively, as main products. Thermolytic studies showed that 2 underwent stepwise decarbonylation to give 3 and 4. All the three products of 2, 3 and 4 were thiolato-bridged dimolybdenum complexes with bond orders of zero, one and two for 2, 3 and 4, respectively. In addition, both 3 and 4 have one and two S atoms bridged in a mu-eta(2)-mode, respectively. The structures of 2 and 3 have been reported previously. The totally decarbonylated 4 was isolated as polymorphs, 4a and 4b, which have been characterized by elemental, spectral analyses and structurally determined. (c) 2007 Elsevier B.V. All rights reserved.
Isolation and characterization of thiolato complexes of [CpCr(SBz)]2S, isomeric trans [CpMo(CO)(SBz)]2 and [CpMo(SBz)2]2 (Cp = (η5-C5H5), Bz = PhCH2) from the reactivity of bibenzyl disulfide towards [CpM(CO)3]2 (M = Cr, Mo)
作者:Mei Lee Ooi、Chu Er Lim、Richard C.S. Wong、Seik Weng Ng
DOI:10.1016/j.ica.2017.08.029
日期:2017.10
Abstract The reactions of [CpM(CO) 3 ] 2 (M = Cr ( 1 ), Mo ( 3 )) with Bz 2 S 2 have been investigated. 1 underwent a facile reaction at ambient temperature which led to the isolation of [CpCr(CO) 2 ]S ( 5 ), [CpCr(CO) 2 (SBz)] 2 ( 6 ) and [CpCr(SBz)] 2 S ( 7 ) in 28.8, 42.6 and 11.8% yield, respectively. A similar reaction at 110 °C with its congener, [CpCr(CO) 2 ] 2 (Cr Cr) ( 2 ) yielded only thermolytic