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Synthesis of diphenyl-(2-thienyl)phosphine, its chalcogenide derivatives and a series of novel complexes of lanthanide nitrates and triflates
Dalton Transactions ( IF 3.5 ) Pub Date : 2022-06-06 , DOI: 10.1039/d2dt01570f Troy Luster 1 , Hannah J Van de Roovaart 1 , Kyle J Korman 1 , Georgia G Sands 1 , Kylie M Dunn 1 , Anthony Spyker 1 , Richard J Staples 2 , Shannon M Biros 1 , John E Bender 1
Dalton Transactions ( IF 3.5 ) Pub Date : 2022-06-06 , DOI: 10.1039/d2dt01570f Troy Luster 1 , Hannah J Van de Roovaart 1 , Kyle J Korman 1 , Georgia G Sands 1 , Kylie M Dunn 1 , Anthony Spyker 1 , Richard J Staples 2 , Shannon M Biros 1 , John E Bender 1
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A novel synthesis of diphenyl(2-thienyl)phosphine, along with its’ oxide, sulfide and selenide derivatives, is reported here. These phosphines have been characterized by NMR, IR, MS and X-Ray crystallography. The phosphine oxide derivative was reacted with a selection of lanthanide(III) nitrates and triflates, LnX3, to give the resultant metal–ligand complexes. These complexes have also been characterized by NMR, IR, MS and X-Ray crystallography. Single crystal X-Ray diffraction data shows a difference in metal–ligand complex stoichiometry and stereochemistry depending on the counteranion (nitrate vs. triflate). The [Ln(Ar3P![[double bond, length as m-dash]](https://www.rsc.org/images/entities/char_e001.gif)
O)3(NO3)3] ligand–nitrate complexes are nine-coordinate to the metal in the solid state (bidentate nitrate), featuring a 1 : 3 lanthanide–ligand ratio and bear an overall octahedral arrangement of the six, coordinated ligands. Our [Ln(Ar3PO)3(NO3)3] ligand–nitrate complexes gave three examples of fac-stereochemistry, where mer-stereochemistry is almost universally observed in the literature of highly related [Ln(Ar3PO)3(NO3)3] complexes. For the Tb complexes, two different arrangements of the ligands around the metal were observed in the solid state for [Tb(Ar3PO)3(NO3)3] and [Tb(Ar3PO)4(OTf)2] [OTf]. [Tb(Ar3PO)3(NO3)3] is strictly nine-coordinate, ligand mer-stereochemistry in the solid state, and [Tb(Ar3PO)4(OTf)2] [OTf] is strictly octahedral, six-coordinate, with a square-planar stereochemical arrangement of the phosphine oxide ligands around the metal.
中文翻译：
二苯基-(2-噻吩基)膦及其硫属化物衍生物及一系列新型镧系硝酸盐和三氟甲磺酸盐配合物的合成
本文报道了二苯基 (2-噻吩基) 膦及其氧化物、硫化物和硒化物衍生物的新合成方法。这些膦已通过 NMR、IR、MS 和 X 射线晶体学进行了表征。氧化膦衍生物与选择的镧系元素 ( III ) 硝酸盐和三氟甲磺酸盐 LnX 3反应，得到生成的金属-配体配合物。这些配合物也已通过 NMR、IR、MS 和 X 射线晶体学进行了表征。单晶 X 射线衍射数据显示金属-配体复合物化学计量和立体化学的差异取决于抗衡阴离子（硝酸根与三氟甲磺酸根）。[Ln(Ar 3 PO) 3 (NO 3 ) 3] 配体 - 硝酸盐配合物与固态金属（硝酸二齿）具有九配位，具有 1:3 的镧系元素 - 配体比例，并具有六个配体的整体八面体排列。我们的 [Ln(Ar 3 P O) 3 (NO 3 ) 3 ] 配体-硝酸盐配合物给出了三个fac立体化学的例子，其中mer立体化学在高度相关的 [Ln(Ar 3 P O)文献中几乎普遍观察到。 3 (NO 3 ) 3 ] 配合物。对于 Tb 配合物，在固态下观察到金属周围配体的两种不同排列 [Tb(Ar3 PO) 3 (NO 3 ) 3 ]和[Tb(Ar 3 PO) 4 (OTf) 2 ] [OTf]。[Tb(Ar 3 PO) 3 (NO 3 ) 3 ]是严格的九配位体，固态配体mer-立体化学，[Tb(Ar 3 P O) 4 (OTf) 2 ] [OTf]是严格的八面体，六配位，金属周围的氧化膦配体呈方形平面立体化学排列。
更新日期：2022-06-06
O)3(NO3)3] ligand–nitrate complexes are nine-coordinate to the metal in the solid state (bidentate nitrate), featuring a 1 : 3 lanthanide–ligand ratio and bear an overall octahedral arrangement of the six, coordinated ligands. Our [Ln(Ar3PO)3(NO3)3] ligand–nitrate complexes gave three examples of fac-stereochemistry, where mer-stereochemistry is almost universally observed in the literature of highly related [Ln(Ar3PO)3(NO3)3] complexes. For the Tb complexes, two different arrangements of the ligands around the metal were observed in the solid state for [Tb(Ar3PO)3(NO3)3] and [Tb(Ar3PO)4(OTf)2] [OTf]. [Tb(Ar3PO)3(NO3)3] is strictly nine-coordinate, ligand mer-stereochemistry in the solid state, and [Tb(Ar3PO)4(OTf)2] [OTf] is strictly octahedral, six-coordinate, with a square-planar stereochemical arrangement of the phosphine oxide ligands around the metal.
中文翻译：
二苯基-(2-噻吩基)膦及其硫属化物衍生物及一系列新型镧系硝酸盐和三氟甲磺酸盐配合物的合成
本文报道了二苯基 (2-噻吩基) 膦及其氧化物、硫化物和硒化物衍生物的新合成方法。这些膦已通过 NMR、IR、MS 和 X 射线晶体学进行了表征。氧化膦衍生物与选择的镧系元素 ( III ) 硝酸盐和三氟甲磺酸盐 LnX 3反应，得到生成的金属-配体配合物。这些配合物也已通过 NMR、IR、MS 和 X 射线晶体学进行了表征。单晶 X 射线衍射数据显示金属-配体复合物化学计量和立体化学的差异取决于抗衡阴离子（硝酸根与三氟甲磺酸根）。[Ln(Ar 3 P
O) 3 (NO 3 ) 3] 配体 - 硝酸盐配合物与固态金属（硝酸二齿）具有九配位，具有 1:3 的镧系元素 - 配体比例，并具有六个配体的整体八面体排列。我们的 [Ln(Ar 3 P O) 3 (NO 3 ) 3 ] 配体-硝酸盐配合物给出了三个fac立体化学的例子，其中mer立体化学在高度相关的 [Ln(Ar 3 P O)文献中几乎普遍观察到。 3 (NO 3 ) 3 ] 配合物。对于 Tb 配合物，在固态下观察到金属周围配体的两种不同排列 [Tb(Ar3 PO) 3 (NO 3 ) 3 ]和[Tb(Ar 3 PO) 4 (OTf) 2 ] [OTf]。[Tb(Ar 3 PO) 3 (NO 3 ) 3 ]是严格的九配位体，固态配体mer-立体化学，[Tb(Ar 3 P O) 4 (OTf) 2 ] [OTf]是严格的八面体，六配位，金属周围的氧化膦配体呈方形平面立体化学排列。
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