2013
DOI: 10.1002/ejic.201300943
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NaRb7(Si4–xGex)2 – Soluble Zintl Phases Containing Heteroatomic Tetrahedral ­[Si4–xGex]4– Clusters

Abstract: A sequential CH functionalization strategy for the synthesis of the marine alkaloid dictyodendrin B is reported. Our synthesis begins from commercially available 4‐bromoindole and involves six direct functionalizations around the heteroarene core as part of a gram‐scale strategy towards the natural product.

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Cited by 14 publications
(10 citation statements)
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“…The results from FPLO and Wien2k for the calculated DOS were qualitatively identical showing the same contributions as already reported in Rb 7 NaSi 8 . [21] Comparison of QM calculated with experimentally determined NMR coupling parameters from previous studies on intermetallic phases -MGa 2 (M = Ca, Sr, and Ba) , [13] MGa 4 (M = Na, Ca, Sr, and Ba), [14] M 4 Si 4 (M = Na, Rb, K, and Cs) [20] as well as Ba 2 Si 4 [12] and Rb 7 NaSi 8 [21] and NaRb 7 (Si 4-x Ge x ) 2 [22] -indicates that a good agreement can be achieved within the following ranges: Ϯ 10 ppm for the NMR signal shift and shift anisotropy, Ϯ 0.1 MHz for C Q and Ϯ0.1 ϫ 10 21 V m -2 for V ZZ , respectively. In case of asymmetry parameters η ϶ 0, an error of Ϯ 0.05 can be estimated.…”
Section: Qm Calculation Procedures: Qtaim Eli and Dosmentioning
confidence: 99%
See 1 more Smart Citation
“…The results from FPLO and Wien2k for the calculated DOS were qualitatively identical showing the same contributions as already reported in Rb 7 NaSi 8 . [21] Comparison of QM calculated with experimentally determined NMR coupling parameters from previous studies on intermetallic phases -MGa 2 (M = Ca, Sr, and Ba) , [13] MGa 4 (M = Na, Ca, Sr, and Ba), [14] M 4 Si 4 (M = Na, Rb, K, and Cs) [20] as well as Ba 2 Si 4 [12] and Rb 7 NaSi 8 [21] and NaRb 7 (Si 4-x Ge x ) 2 [22] -indicates that a good agreement can be achieved within the following ranges: Ϯ 10 ppm for the NMR signal shift and shift anisotropy, Ϯ 0.1 MHz for C Q and Ϯ0.1 ϫ 10 21 V m -2 for V ZZ , respectively. In case of asymmetry parameters η ϶ 0, an error of Ϯ 0.05 can be estimated.…”
Section: Qm Calculation Procedures: Qtaim Eli and Dosmentioning
confidence: 99%
“…Recent studies on the alkali metal silicides M 4 Si 4 [20] with M = Na, K, Rb, Cs and Ba 2 Si 4 as well as Rb 7 NaSi 8 [21] and NaRb 7 (Si 4-x Ge x ) 2 [22] promote the analysis of chemical bonding using both, experimental and theoretical methods for this fascinating class of Zintl phases. [23,24] The undertakings to study the influence of different cations on the chemical bonding of the common structural feature of Si 4 4-cluster-anions in binary alkali metal silicides led to the investigation of the ternary phase Rb 7 NaSi 8 .…”
Section: Introductionmentioning
confidence: 99%
“…The cocrystallization of mesitylene in 4 and the presence of [MesCuMes] À (5 a) in 5 provides strong evidence that the migration of a bare Cu atom into an Sn 9 anion takes place through the release of a Mes À anion from mesitylcopper, which either migrates to another mesitylcopper to form 5 a or is subsequently protonated to give MesH.Zintl phases of the type A 4 E 9 and A 12 E 17 (A = K-Cs and E = Si-Pb), which contain exclusively nona-atomic [E 9 ] 4À or simultaneously [E 9 ] 4À and [E 4 ] 4À cluster anions, respectively, react in liquid ammonia, ethylenediamine (en), or N,N-dimethylformamide (dmf) with transition-metal complexes in two different manners: One possibility is that the clusters themselves act as sor p-bonded ligands. [1] In the case of nine-atomic cluster compounds, a large variety of different complexes of this type have been reported, such as [(h 4 -Si 9 )ZnPh] 3À , [2] [(h 4 -Ge 9 )CuPiPr 3 ] 3À , [3] [(h 4 -Sn 9 )Cr(CO) 3 ] 4À , [4] [(h 4 -Sn 9 )Ir(cod)] 3À (cod = cyclooctadiene), [5] [(h 4 -Pb 9 )M(CO) 3 ] 4À (M = Mo, W), [6] [(h 1 -Si 9 ) 2 {Ni(CO) 2 } 2 ] 8À , [7] [(h 4 -Ge 9 )Cu(h 1 -Ge 9 )] 7À , [3] [(Ge 9 )Au 3 (Ge 9 )] 5À , [8] [Au 3 Ge 45 ] 9À , [9] or [Ag(Sn 9 ÀSn 9 )] 5À , [10] whereas only a limited number of complexes of tetrahedral clusters, such as [(MesCu) 2 (h 3 -E 4 )] 4À (E = Si, Ge), [11,12] mixed clusters in [(MesCu) 2 -(Si 4Àx Ge x )] 4À (x = 2.2(1)) [13] and [(h 2 -Sn 4 )Zn(h 3 -Sn 4 )] 6À[14] , are known. Recently, neat E 4 clusters (E = Si, Sn) have been characterized by 29 Si and 119 Sn NMR spectroscopy [15] and isolated as solvates, for example, in the compounds A 4 Sn 4 ·(NH 3 ) 2 (A = Rb, Cs), Rb 4 Pb 4 ·(NH 3 ) 2 , [16] and Na 4 Sn 4 ·(NH 3 ) 13 , [17] which offer new access to subsequent reactions of these clusters in solution.The second variant is that these clusters incorporate a transition metal, leading to the formation of endohedral cluster subunits.…”
mentioning
confidence: 99%
“…In addition, it was possible to monitor the synthesis of alkyl‐capped Si nanoparticles from Na 4 Si 4 and SiCl 4 by NMR spectroscopy . Furthermore, the binary compounds A 4 T 4 , A 4 Ge 9 , and A 12 T 17 are frequently used as precursors for the preparation and modification of Zintl clusters in solution , …”
Section: Introductionmentioning
confidence: 99%
“…Some of us have recently applied this approach to gain insights into the chemical bonding in the Zintl phases A 4 Si 4 ( A = Na–Cs) and A 7 NaSi 8 ( A = Rb, Cs), which all contain tetrahedral [Si 4 ] 4– clusters , , . In the solid solutions Rb 7 NaSi 8– x Ge x , the presence of mixed (Si 4– x Ge x ) 4– clusters could be proven by using these techniques …”
Section: Introductionmentioning
confidence: 99%