An Organometallic Radical Route to Bis(phosphido)- and Hydrido−Phosphido-Bridged Metal−Metal-Bonded Complexes of Cyclopentadienylchromium via Desulfurization of Thiophosphinito Ligands
An Organometallic Radical Route to Bis(phosphido)- and Hydrido−Phosphido-Bridged Metal−Metal-Bonded Complexes of Cyclopentadienylchromium via Desulfurization of Thiophosphinito Ligands
复制标题
通过硫代膦配体脱硫生成环戊二烯基铬双(磷基)-和氢磷基-桥金属-金属键配合物的有机金属路线
DOI：
--
复制
发表时间：
2002
期刊：
影响因子：
--
通讯作者：
I. Haiduc
中科院分区：
文献类型：
--
作者：
L. Goh;Z. Weng;W. Leong;J. Vittal;I. Haiduc
[CpCr（CO）3]2（1，Cp = η5-C5 H5）与1摩尔当量的四烷基二膦二硫化物R2 P（S）P（S）R2（R = Me，Et）在60 °C下反应24小时，导致分离出硫代亚膦基络合物CpCr（CO）2（SPR 2）（2a，R = Me; 2b，R = Et），为暗红色固体，在约100 ° C下。24%的收益。用有机金属基CpCr（CO）3·（1A）脱硫2a，得到双（μ-膦基）金属-金属双键配合物Cp 2Cr 2（CO）4（μ-H）（μ-PMe 2）（3a），双（μ-膦基）金属-金属双键配合物Cp 2Cr 2（CO）2（μ-PMe 2）2（4a）和三角三核配合物Cp 3Cr 3（CO）3（S）（PMe 2）（5a）。通过单晶X射线衍射分析确定了所有配合物的固态结构。
The reaction of [CpCr(CO)3]2 (1, Cp = η5-C5H5) with 1 mol equiv of the tetraalkyldiphosphine disulfide R2P(S)P(S)R2 (R = Me, Et) at 60 °C for 24 h led to the isolation of the thiophosphinito complexes CpCr(CO)2(SPR2) (2a, R = Me; 2b, R = Et) as dark red solids in ca. 24% yield. Desulfurization of 2a by the organometallic radical CpCr(CO)3• (1A) gave the hydrido−phosphido-bridged complex Cp2Cr2(CO)4(μ-H)(μ-PMe2) (3a), the bis(μ-phosphido) metal−metal doubly bonded complex Cp2Cr2(CO)2(μ-PMe2)2 (4a), and the triangulo trinuclear complex Cp3Cr3(CO)3(S)(PMe2) (5a). The solid-state structures of all of the complexes have been determined by single-crystal X-ray diffraction analysis.