Stannylplumbylenes: bonding between tetravalent tin and divalent lead

Drost, Christian; Lönnecke, Peter; Sieler, Joachim

doi:10.1039/c2cc30687e

Cited by 9 publications

(11 citation statements)

References 41 publications

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“…In the case of the lead halide, a plumbylene was synthesized which shows a resonance in the 207 Pb NMR spectrum at typical low field of 8885 ppm indicating a monomeric plumbylene structure in solution: 82 [Ar 3 SnPbAr] ( 207 Pb, 6905 ppm) and [(Ar 3 Sn) 2 Pb] ( 207 Pb, 7853 ppm) (Ar = C 6 H 3 (OiPr) 2 -2,6). 82 The SnH 2 unit of 10 exhibits in the 1 H NMR spectrum (16.42 ppm), as well as in the 119 Sn NMR spectrum (1199 ppm), a signal for a tetracoordinate tin atom at very low field. In comparison trip 2 SnH 2 shows signals at 6.33 ( 1 H NMR) and −352.1 ppm ( 119 Sn NMR).…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…73,74 Low field 119 Sn NMR chemical shifts were also observed in the case of plumbylenes [Ar 3 SnPbAr] ( 119 Sn, 1270 ppm; 207 Pb, 6905 ppm) and [(Ar 3 Sn) 2 Pb] ( 119 Sn, 1273 ppm; 207 Pb, 7853 ppm) (Ar = C 6 H 3 (OiPr) 2 -2,6). 82 In the solid-state structure of stannylplumbylene 10 (Figure 5), we found a Sn−Pb distance of 2.90767 (15) Å which lies in the range of literature examples: [Ar 3 SnPbAr] 2.8784(4), [(Ar 3 Sn) 2 Pb] 2.9283(4), 2.9483(6) Å. 82,86,87 Formation of 10 was also found in reaction between low-valent organohydrides of tin and lead.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

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Deprotonation of Organogermanium and Organotin Trihydrides

et al. 2019

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Terphenyltin and terphenylgermanium trihydrides were deprotonated in reaction with strong bases, such as LiMe, LDA, or KBn. In the solid state, the Li salts of the germate anion 4 and 4a exhibit a Li–Ge contact. In the Li salt of the dihydridostannate anion 6a, the Li cation is not coordinated at the tin atom instead an interaction of the Li cation with the hydride substituents was found. Evidenced by 1H–7Li-HOESY NMR spectroscopy the Li-salt of the deprotonated tin hydride 6a exhibits in toluene solution a contact between Li cation and hydride substituents, whereas in the 1H–7Li-HOESY NMR spectrum of the homologous germate salt 4a, no crosspeak between hydride and Li signals was found. The organodihydridogermate and -stannate react as nucleophiles with low-valent Group 14 electrophiles. Thus, three compounds were synthesized: Ar–Ë′–EH2–Ar (E′, E = Sn, Ge; Pb, Ge; Pb, Sn; Ar = Ar′, Ar*). Following an alternative synthesis Ar′SnH2PbAr* was synthesized in reaction between [(Ar*PbH)2] and [(Ar′SnH)4] generated in situ. In reaction between low-valent organotin hydride [(Ar*SnH)2] and organdihydridostannate [Ar*SnH2]− formation of distannate [Ar*2Sn2H3]− was found.

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Section: ■ Results and Discussionmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Deprotonation of Organogermanium and Organotin Trihydrides

et al. 2019

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“…870 ppm compared to the three-coordinate tin(II) atom in 1 (δ =´191 ppm). The 207 Pb NMR spectrum of 3 is characterized by one signal at´1643 ppm and a 1 J( 207 Pb-119/117 Sn) coupling of 14900 Hz, which is smaller than observed for the hitherto isolated stannylplumbylenes (19971-22560 Hz) [26], but larger than determined for stannylplumbanes, e.g., Ph 3 SnPbPh 3 (3469 Hz) [33,34]. The chemical shift value of the three-coordinate lead atom in 3, however, is strikingly deviating from low field 207 Pb resonances usually observed for triaryl plumbates, e.g., at +1063 ppm for LiPbPh 3 [35] or +1020 ppm for the related [LiPb(2-py 6OtBu ) 3 ] [36].…”

Section: Resultsmentioning

confidence: 99%

“…Similar structural features can be found in the previously reported tris(plumbyl)plumbate anions, where angles around the central lead atom average to 93.0˝ [11] and 94.1˝ [12]. The Pb-Sn bond lengths amount to 2.8743(3) and 2.8919(4) Å, and may be compared with 2.7844(4) Å in Pb(Ar)SnAr 3 (Ar = C 6 H 3 -2,6-(O i Pr) 2 ) and 2.9283(4) Å in Pb(SnAr 3 ) 2 [26].…”

Section: Resultsmentioning

confidence: 99%

Monoanionic Tin Oligomers Featuring Sn–Sn or Sn–Pb Bonds: Synthesis and Characterization of a Tris(Triheteroarylstannyl)Stannate and -Plumbate

Zeckert

2016

Inorganics

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Abstract:The reaction of the lithium tris(2-pyridyl)stannate [LiSn(2-py 6OtBu ) 3 ] (py 6OtBu = C 5 H 3 N-6-OtBu), 1, with the element(II) amides E{N(SiMe 3 ) 2 } 2 (E = Sn, Pb) afforded complexes [LiE{Sn(2-py 6OtBu ) 3 } 3 ] for E = Sn (2) and E = Pb (3), which reveal three Sn-E bonds each. Compounds 2 and 3 have been characterized by solution NMR spectroscopy and X-ray crystallographic studies. Large 1 J( 119 Sn-119/117 Sn) as well as 1 J( 207 Pb-119/117 Sn) coupling constants confirm their structural integrity in solution. However, contrary to 2, complex 3 slowly disintegrates in solution to give elemental lead and the hexaheteroarylditin [Sn(2-py 6OtBu ) 3 ] 2 (4).

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“…67 A diplumbylene is formed in the reaction of potassium {1,1,4,4,-(SiMe 3 ) 4 -2,2,3,3-(Me) 4 -tetrasilane} with lead(II) bromide in the presence of triethylphosphine, giving initially [{1,1,4,4,-(SiMe 3 ) 4 -2,2,3,3-(Me) 4 -tetrasilane}]Pb(PEt 3 ) (2) that loses the phosphine upon reaction with Massey's (perfluoro)triphenylboron to produce the dimer ([{1,1,4,4,-(SiMe 3 ) 4 -2,2,3,3-(Me) 4 -tetrasilane}]Pb) 2 (…”

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confidence: 99%