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Cyclopentadienylidene- and Fluoren-9-ylidene-methane-1,1-dithiolato Metalates of Tin, Indium and Bismuth
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2021-08-26 , DOI: 10.1002/ejic.202100570 Tobias Vollgraff 1 , Nick Michel 1 , Jörg Sundermeyer 2
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2021-08-26 , DOI: 10.1002/ejic.202100570 Tobias Vollgraff 1 , Nick Michel 1 , Jörg Sundermeyer 2
Affiliation
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Quaternary ammonium and phosphonium stannates(II), indates(III) and bismuthates(III) displaying dianionic S,S dithiolate chelate ligands [CpCS2]2− and [FluoCS2]2− (Cp=C5H4, Fluo=C13H8) are described. With Sn(II) as central template ion, homoleptic metalates Cat2[Sn(CpCS2)2], with In(III) and Bi(III), highly charged Cat3[In(CpCS2)3] and Cat3[Bi(CpCS2)3] were obtained. A complementary series was characterized for fluoren-9-ylidene-derived metalates Cat2[(FluoCS2)2Sn], Cat3[(FluoCS2)3In] and Cat3[Bi(FluoCS2)3]. Heteroleptic indate(III) NBu4[CpCS2InMe2] (3-NBu4) and homoleptic [PPh4]3[In(CpCS2)3] (6-PPh4) as well as stannates(II) [PPh4]2[Sn(CpCS2)2] (5-PPh4) and [NBu4]2[Sn(FluoCS2)2] (9-NBu4) were XRD structurally characterized. Reaction of electron-rich ligand Na2(FluoCS2) with SnCl4 did not lead to an expected stannate(IV) but to a redox reaction and metal free 3,5-di(9H-fluorene-9-ylidene)-1,2,4-trithiolane (12), which was characterized by XRD analysis. The title compounds are related to much better investigated dithiocarbamato(2-) complexes, well-established precursors for thermal metal sulfide depositions. In this respect, an explorative DSC-TGA measurement following the thermal decay of [PPh4]3[(CpCS2)3In] (6-PPh4) revealed the formation of β-In2S3 at relatively high temperatures, proven by PXRD.
中文翻译：
锡、铟和铋的环戊二烯基和芴-9-ylidene-methane-1,1-dithiolato 金属盐
季铵和鏻锡酸盐 (II)、茚酸 (III) 和铋酸盐 (III) 显示双阴离子S,S 二硫醇螯合物配体 [CpCS 2 ] 2−和 [FluoCS 2 ] 2− (Cp=C 5 H 4 , Fluo=C 13 H 8 ) 进行了描述。以 Sn(II) 作为中心模板离子，均质金属化 Cat 2 [Sn(CpCS 2 ) 2 ]、In(III) 和 Bi(III)、高电荷 Cat 3 [In(CpCS 2 ) 3 ] 和 Cat 3 [ Bi(CpCS 2 ) 3] 获得。对芴-9-亚基衍生的金属化物 Cat 2 [(FluoCS 2 ) 2 Sn]、Cat 3 [(FluoCS 2 ) 3 In] 和 Cat 3 [Bi(FluoCS 2 ) 3 ]的互补系列进行了表征。杂配的铟酸盐(III) NBu 4 [CpCS 2 InMe 2 ] ( 3-NBu 4 ) 和杂配的 [PPh 4 ] 3 [In(CpCS 2 ) 3 ] ( 6-PPh 4 ) 以及锡酸盐(II) [PPh 4 ] 2 [Sn(CpCS2 ) 2 ] ( 5-PPh 4 ) 和[NBu 4 ] 2 [Sn(FluoCS 2 ) 2 ] ( 9-NBu 4 ) 进行XRD 结构表征。富电子配体 Na 2 (FluoCS 2 ) 与 SnCl 4 的反应没有产生预期的锡酸盐 (IV)，而是产生氧化还原反应和不含金属的 3,5-di(9 H -芴-9-亚基)-1 ,2,4-三硫戊烷 ( 12)，通过 XRD 分析对其进行表征。标题化合物与更好研究的二硫代氨基甲酸 (2-) 配合物有关，它们是用于热金属硫化物沉积的成熟前体。在这方面，在 [PPh 4 ] 3 [(CpCS 2 ) 3 In] ( 6-PPh 4 )热衰变之后的探索性 DSC-TGA 测量揭示了β -In 2 S 3在相对较高的温度下的形成，证明通过 PXRD。
更新日期：2021-10-01
中文翻译：
锡、铟和铋的环戊二烯基和芴-9-ylidene-methane-1,1-dithiolato 金属盐
季铵和鏻锡酸盐 (II)、茚酸 (III) 和铋酸盐 (III) 显示双阴离子S,S 二硫醇螯合物配体 [CpCS 2 ] 2−和 [FluoCS 2 ] 2− (Cp=C 5 H 4 , Fluo=C 13 H 8 ) 进行了描述。以 Sn(II) 作为中心模板离子，均质金属化 Cat 2 [Sn(CpCS 2 ) 2 ]、In(III) 和 Bi(III)、高电荷 Cat 3 [In(CpCS 2 ) 3 ] 和 Cat 3 [ Bi(CpCS 2 ) 3] 获得。对芴-9-亚基衍生的金属化物 Cat 2 [(FluoCS 2 ) 2 Sn]、Cat 3 [(FluoCS 2 ) 3 In] 和 Cat 3 [Bi(FluoCS 2 ) 3 ]的互补系列进行了表征。杂配的铟酸盐(III) NBu 4 [CpCS 2 InMe 2 ] ( 3-NBu 4 ) 和杂配的 [PPh 4 ] 3 [In(CpCS 2 ) 3 ] ( 6-PPh 4 ) 以及锡酸盐(II) [PPh 4 ] 2 [Sn(CpCS2 ) 2 ] ( 5-PPh 4 ) 和[NBu 4 ] 2 [Sn(FluoCS 2 ) 2 ] ( 9-NBu 4 ) 进行XRD 结构表征。富电子配体 Na 2 (FluoCS 2 ) 与 SnCl 4 的反应没有产生预期的锡酸盐 (IV)，而是产生氧化还原反应和不含金属的 3,5-di(9 H -芴-9-亚基)-1 ,2,4-三硫戊烷 ( 12)，通过 XRD 分析对其进行表征。标题化合物与更好研究的二硫代氨基甲酸 (2-) 配合物有关，它们是用于热金属硫化物沉积的成熟前体。在这方面，在 [PPh 4 ] 3 [(CpCS 2 ) 3 In] ( 6-PPh 4 )热衰变之后的探索性 DSC-TGA 测量揭示了β -In 2 S 3在相对较高的温度下的形成，证明通过 PXRD。
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