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Rh(I)(2,5-norbornadiene)(biphenyl)(tris(4-fluorophenyl)phosphine): Synthesis, Characterization, and Application as an Initiator in the Stereoregular (Co)Polymerization of Phenylacetylenes
ACS Macro Letters ( IF 5.1 ) Pub Date : 2019-12-24 , DOI: 10.1021/acsmacrolett.9b00975 Nicholas Sheng Loong Tan 1 , Gareth L Nealon 2 , Gemma F Turner 2 , Stephen A Moggach 2 , Mark I Ogden 1 , Massimiliano Massi 1 , Andrew B Lowe 1
ACS Macro Letters ( IF 5.1 ) Pub Date : 2019-12-24 , DOI: 10.1021/acsmacrolett.9b00975 Nicholas Sheng Loong Tan 1 , Gareth L Nealon 2 , Gemma F Turner 2 , Stephen A Moggach 2 , Mark I Ogden 1 , Massimiliano Massi 1 , Andrew B Lowe 1
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The synthesis of the Rh(I)-aryl complex, Rh(I)(nbd)(BiPh)(P(4-FC6H4)3) is reported and its efficacy as an initiator for the (co)polymerization of phenylacetylenes established. The X-ray crystal structure indicates that the complex adopts a slightly distorted square planar geometry whose purity and structure was also confirmed by elemental analysis and 1H, 13C, 31P, 19F, 103Rh, and 31P-103Rh{1H} HMQC NMR spectroscopy. We demonstrate that Rh(I)(nbd)(BiPh)(P(4-FC6H4)3) mediates the (co)polymerization of phenylacetylenes in a controlled fashion with initiation efficiencies as high as 0.98, as evidenced by the pseudo-first-order kinetic and number-average molecular weight versus conversion profiles. The ability to form well-defined AB diblock copolymers, in a stereoregular manner, by sequential monomer addition is verified in the block copolymerization of phenylacetylene with 4-fluorophenylacetylene with quantitative crossover efficiency, as determined by size exclusion chromatography.
中文翻译：
Rh(I)(2,5-norbornadiene)(biphenyl)(tris(4-fluorophenyl)phosphine)：合成、表征和作为引发剂在苯乙炔的立体定向 (Co) 聚合中的应用
报道了Rh(I)-芳基配合物Rh(I)(nbd)(BiPh)(P(4-FC 6 H 4 ) 3 )的合成及其作为苯乙炔(共)聚合引发剂的功效已确立的。X 射线晶体结构表明该配合物采用略微扭曲的方形平面几何形状，其纯度和结构也通过元素分析和1 H、13 C、31 P、19 F、103 Rh 和31 P- 103 Rh{ 1 H} HMQC NMR光谱。我们证明了Rh(I)(nbd)(BiPh)(P(4-FC 6 H 4 ) 3) 以受控方式介导苯乙炔的（共）聚合，引发效率高达 0.98，伪一级动力学和数均分子量与转化曲线的关系证明了这一点。在苯乙炔与 4-氟苯乙炔的嵌段共聚中，通过尺寸排阻色谱法测定，通过顺序单体添加以有规立构的方式形成明确定义的 AB 二嵌段共聚物的能力得到了验证，具有定量的交叉效率。
更新日期：2019-12-25
中文翻译：
Rh(I)(2,5-norbornadiene)(biphenyl)(tris(4-fluorophenyl)phosphine)：合成、表征和作为引发剂在苯乙炔的立体定向 (Co) 聚合中的应用
报道了Rh(I)-芳基配合物Rh(I)(nbd)(BiPh)(P(4-FC 6 H 4 ) 3 )的合成及其作为苯乙炔(共)聚合引发剂的功效已确立的。X 射线晶体结构表明该配合物采用略微扭曲的方形平面几何形状，其纯度和结构也通过元素分析和1 H、13 C、31 P、19 F、103 Rh 和31 P- 103 Rh{ 1 H} HMQC NMR光谱。我们证明了Rh(I)(nbd)(BiPh)(P(4-FC 6 H 4 ) 3) 以受控方式介导苯乙炔的（共）聚合，引发效率高达 0.98，伪一级动力学和数均分子量与转化曲线的关系证明了这一点。在苯乙炔与 4-氟苯乙炔的嵌段共聚中，通过尺寸排阻色谱法测定，通过顺序单体添加以有规立构的方式形成明确定义的 AB 二嵌段共聚物的能力得到了验证，具有定量的交叉效率。
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