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Sandwich and Half-Sandwich Ln(II) (Ln = Sm, Yb) Complexes with Bulky Fluorenyl Ligands. Competitive Abstraction of H or SiMe3 from 2,7-tBu2-9-SiMe3-Fluorene by an Amido Anion
Organometallics ( IF 2.8 ) Pub Date : 2021-08-23 , DOI: 10.1021/acs.organomet.1c00406 Alexander N. Selikhov 1, 2 , Ivan V. Lapshin 1 , Anton V. Cherkasov 1 , Georgy K. Fukin 1 , Alexander A. Trifonov 1, 2
Organometallics ( IF 2.8 ) Pub Date : 2021-08-23 , DOI: 10.1021/acs.organomet.1c00406 Alexander N. Selikhov 1, 2 , Ivan V. Lapshin 1 , Anton V. Cherkasov 1 , Georgy K. Fukin 1 , Alexander A. Trifonov 1, 2
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The half-sandwich fluorenyl-amido complex [2,7-tBu2-9-SiMe3C13H6]Yb[N(SiMe3)2](DME) was synthesized by the reaction of [(Me3Si)2N]2Yb(THF)2 with 2,7-tBu2-9-SiMe3C13H7 (1:1 molar ratio) in 83% yield. The analogous reaction of [(Me3Si)2N]2Sm(THF)2 affords a mixture of equimolar amounts of the half-sandwich complexes [2,7-tBu2-9-SiMe3C13H6]Sm[N(SiMe3)2](DME) (2a) and heteroligand sandwich [2,7-tBu2-9-SiMe3C13H6]Sm[2,7-tBu2C13H7](DME) (2b). The heteroligand sandwich complex [2,7-tBu2-9-SiMe3C13H6]Sm[2,7-tBu2-C13H7](THF)2 (3) was synthesized in 60% yield by reacting [(Me3Si)2N]2Sm(THF)2 with 2 equiv of 2,7-tBu2-9-SiMe3C13H7. Complexes 2b and 3 result from competitive abstraction of H or SiMe3 from 2,7-tBu2-9-SiMe3-fluorene by an amido group. In contrast, the homoligand sandwich complex [2,7-tBu2-9-SiMe3C13H6]2Sm(DME) (5) could be synthesized in 80% yield when [(p-tBuC6H4)2 CH]2Sm(DME)2 was used as a precursor. The complex (2,7-tBu2C13H7)2Sm(THF)2 (6) was synthesized by the reaction of 2,7-tBu2C13H8 with [(Me3Si)2N]2Sm(THF)2 (2:1) in 65% yields. The crystal structures of complexes 1, 2a,b, 3, 5, and 6 were established by X-ray analyses.
中文翻译：
夹心和半夹心 Ln(II) (Ln = Sm, Yb) 与大块芴基配体的复合物。通过酰胺阴离子从 2,7-tBu2-9-SiMe3-芴中竞争性提取 H 或 SiMe3
半夹心芴基酰氨基配合物[2,7-吨卜2 -9-森达3 Ç 13 ħ 6 ]的Yb [N（森达3）2 ]（DME）中的溶液通过反应合成[（ME 3 Si）的2 N] 2 Yb(THF) 2与2,7 - t Bu 2 -9-SiMe 3 C 13 H 7 (1:1 摩尔比)，产率为 83%。[(Me 3 Si) 2 N] 2 Sm(THF) 2的类似反应得到等摩尔量的半夹心配合物[2,7-t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm[N(SiMe 3 ) 2 ](DME) ( 2a ) 和杂配体夹层 [2,7- t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm [2,7- t Bu 2 C 13 H 7 ](DME) ( 2b )。杂配体夹心复合物 [2,7- t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm[2,7- t Bu 2 -C 13H 7 ](THF) 2 ( 3 ) 通过 [(Me 3 Si) 2 N] 2 Sm(THF) 2与 2 当量的 2,7 - t Bu 2 -9-SiMe 3 C反应以 60% 的产率合成13小时7。配合物2b和3是由酰胺基从2,7 - t Bu 2 -9-SiMe 3 -芴竞争性提取H或SiMe 3产生的。相比之下，同源夹心复合物 [2,7- t Bu 2 -9-SiMe 3 C当[( p - t BuC 6 H 4 ) 2 CH] 2 Sm(DME) 2用作前体时，可以以80%的产率合成13 H 6 ] 2 Sm(DME) ( 5 ) 。配合物(2,7- t Bu 2 C 13 H 7 ) 2 Sm(THF) 2 ( 6 )由2,7- t Bu 2 C 13 H 8与[(Me 3 Si) 2 N反应合成。] 2Sm(THF) 2 (2:1) 的产率为 65%。复合物的晶体结构1，图2a，b，3，5，和6通过X射线分析来建立。
更新日期：2021-09-13
中文翻译：
夹心和半夹心 Ln(II) (Ln = Sm, Yb) 与大块芴基配体的复合物。通过酰胺阴离子从 2,7-tBu2-9-SiMe3-芴中竞争性提取 H 或 SiMe3
半夹心芴基酰氨基配合物[2,7-吨卜2 -9-森达3 Ç 13 ħ 6 ]的Yb [N（森达3）2 ]（DME）中的溶液通过反应合成[（ME 3 Si）的2 N] 2 Yb(THF) 2与2,7 - t Bu 2 -9-SiMe 3 C 13 H 7 (1:1 摩尔比)，产率为 83%。[(Me 3 Si) 2 N] 2 Sm(THF) 2的类似反应得到等摩尔量的半夹心配合物[2,7-t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm[N(SiMe 3 ) 2 ](DME) ( 2a ) 和杂配体夹层 [2,7- t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm [2,7- t Bu 2 C 13 H 7 ](DME) ( 2b )。杂配体夹心复合物 [2,7- t Bu 2 -9-SiMe 3 C 13 H 6 ]Sm[2,7- t Bu 2 -C 13H 7 ](THF) 2 ( 3 ) 通过 [(Me 3 Si) 2 N] 2 Sm(THF) 2与 2 当量的 2,7 - t Bu 2 -9-SiMe 3 C反应以 60% 的产率合成13小时7。配合物2b和3是由酰胺基从2,7 - t Bu 2 -9-SiMe 3 -芴竞争性提取H或SiMe 3产生的。相比之下，同源夹心复合物 [2,7- t Bu 2 -9-SiMe 3 C当[( p - t BuC 6 H 4 ) 2 CH] 2 Sm(DME) 2用作前体时，可以以80%的产率合成13 H 6 ] 2 Sm(DME) ( 5 ) 。配合物(2,7- t Bu 2 C 13 H 7 ) 2 Sm(THF) 2 ( 6 )由2,7- t Bu 2 C 13 H 8与[(Me 3 Si) 2 N反应合成。] 2Sm(THF) 2 (2:1) 的产率为 65%。复合物的晶体结构1，图2a，b，3，5，和6通过X射线分析来建立。
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