Metal (Li, GeII, GeIII, SnII, and PbII) 2,6-dialkylbenzenethiolates; X-ray crystal structures of Sn(SAr)2(Ar = C6H2But3-2,4,6) and [M(SAr′)2]3(M = Sn or Pb, Ar′= C6H3Pri2-2,6)

Hitchcock, Peter B.; Läppert, Michael F.; Samways, Barry J.; Weinberg, E.

doi:10.1039/c39830001492

Cited by 74 publications

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“…There are short intramolecular non-bonded distances between H36 and C21 and C22: 2.862(3) and 2.920(4) A in 1 and 2.9 13(6) and 2.972 (7) in 2. The Sn-S distances in 1 are intermediate between the short (terminal) Sn-S distance of 2.471(5) and the twq longer (bridging) Sn-S distances of 2.643(4) and 2.583(4) A found for the pyramidally coordinated Sn(l1) centres in trimeric [Sn(SAr1)J3 (see above), but longer than the Sn-S distance of 2.435(1) A found for monomeric Sn(SAr), (Ar = 2,6-diisobutylphenyl) (23). The S--' Sn-s angle of 85.4(1)" reported for Sn(SAr), is less than any angle found in 1.…”

Section: The [Sn(sc6h5)j]-arzionmentioning

confidence: 93%

“…Overall, the four compounds [(C6Hs),As] [M(EC6H,),], (M = Sn(l1) or Pb(ll), E = S or Se) are both isomorphous and isostructural. In contrast the compounds [M(SAr1),13 (M = Sn(l1) or Pb(l1); Ar' = 2,6-diisopropylphenyl) are not isomorphous and are not considered to be isostructural (23).…”

Section: Descriptiorl Of' the Structuresmentioning

confidence: 99%

“…At the outset of our work no X-ray structural data were available for neutral stannous thiolates or selenolates. Very recently, however, the structures of two substituted benzene thiolates of tin(I1) have been reported (23).…”

Section: Introductionmentioning

confidence: 99%

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Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se

Dean¹,

Vittal²,

Payne³

1985

Can. J. Chem.

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Stannous chloride, in solutions containing at least three mole equivalents of NaEC6H5, E = S and Se, forms triligated anions which crystallize readily as the tetraphenylarsonium salts, [(C6H5)4As[Sn(SC6H5)3], 1, and [(C6H5)4As][Sn(SeC6H5)3], 2. The crystals so formed are isomorphous, and their structures have been determined by single crystal X-ray diffractometry techniques. The salts crystallize in the monoclinic space group P21/c, with four formula units in unit cells of dimensions a = 10.760(1), b = 17.515(2), c = 20.247(3) Å, β = 104.71(1)° for 1, and a = 10.885(2), b = 17.587(2), c = 20.612(2) Å, β = 105.47(1)°, for 2. The structures have been refined by full-matrix least-squares techniques on F to agreement factors R = 0.024 (4780 observations with Fo > 3σ(Fo)) for 1, and R = 0.030 (3442 observations with Fo > 3σ(Fo)) for 2. The discrete [Sn(EC6H5)3]− anions are isostructural; the three S or Se atoms form the base of a triangular pyramid whose apex is occupied by the Sn atom. Two Sn—S distances in 1 are 2.532(1) and the third 2.552(1) Å, while in 2 the Sn—Se distances are 2.649(1), 2.650(1), and 2.671(1) Å. Angles at the Sn atom are 89.91(3), 90.55(3), and 96.73(3)° in 1, and 88.74(3), 89.72(3), and 97.27(3)° in 2. In both anions all three phenyl groups adopt a propeller-like conformation and are disposed in equatorial positions above the basal plane of chalcogen atoms. These salts represent the first thiolato- and sele-nolatostannates(II) to be characterized structurally. Tin-119 nmr spectra confirm that the [Sn(EC6H5)3]− ions are the same anionic Sn(II) species recently prepared insitu in solution.

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Section: The [Sn(sc6h5)j]-arzionmentioning

confidence: 93%

Section: Descriptiorl Of' the Structuresmentioning

confidence: 99%

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Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se

Dean¹,

Vittal²,

Payne³

1985

Can. J. Chem.

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“…Important structural data for 1-14 are given in Table 1 which also includes data for the stannylene, Sn(SMes*)2, (24) for comparison. 9 The most notable feature of the structures is that with The essential coplanarity of the central aryl ring of the terphenyl ligand with the SnS2 core structure is apparent in the structure of 11. The average Si-S distance in silylenes 2 (2.137(1) Å) and 3 (2.089(9) Å) are shorter than in 1 (2.158(3) Å) but are closer to those found in Tilley's bisthiolatosilylene platinum complex, trans-(Cy3P)2Pt(H)Si(SEt)2OTf (2.092(4) and 2.074(4) Å).…”

Section: Structures Dithiolatesmentioning

confidence: 99%

Dispersion Forces and Counterintuitive Steric Effects in Main Group Molecules: Heavier Group 14 (Si–Pb) Dichalcogenolate Carbene Analogues with Sub-90° Interligand Bond Angles

et al. 2013

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The synthesis, spectroscopic and structural characterization of an extensive series of acyclic, monomeric tetrylene dichalcogenolates of formula M(ChAr)2 (M = Si, Ge, Sn, Pb; Ch = O, S, or Se; Ar = bulky m-terphenyl ligand) are described. They were found to possess several unusual features-the most notable of which is their strong tendency to display acute interligand, Ch-M-Ch, bond angles that are often well below 90°.Furthermore, and contrary to normal steric expectations, the interligand angles were 2 found to become narrower as the size of the ligand was increased. Experimental and structural data in conjunction with high-level DFT calculations, including corrections for dispersion effects, led to the conclusion that dispersion forces play a key role in stabilizing their acute interligand angles.

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“…Interestingly, the structure is neither polymeric, as in [Pb(SC 6 H 5 ) 2 ] n [9] or [Pb(S-4-CH 3 C 6 H 4 ) 2 ] n , [10] nor trimeric, as in [Pb 3 (S-2,6-iC 3 H 7 C 6 H 3 ) 6 ], [12] but is found to be oligomeric [Pb 10 {S-2,6-(CH 3 ) 2 C 6 H 3 } 20 ] (1). Complex 1 crystallizes in the space group Pbcn with the molecule residing on an inversion center ( Figure 1).…”

Section: Resultsmentioning

confidence: 99%

Four New Lead(II) Thiolate Cluster Complexes – Unexpected Products of a Conventional Synthesis

Eichhöfer¹

2005

Eur J Inorg Chem

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The reaction of Pb(OOCCH3)2·3H2O with 2.1 equiv. of HS‐2,6‐(CH3)2C6H3 in ethanol/water is expected to give [Pb{S‐2,6‐(CH3)2C6H3}2]. However, we obtained an orange powder whose elemental analysis disagrees with that of the expected product and indicates small amounts of oxygen. Layering of concentrated solutions of this orange powder in dry THF with pentane under nitrogen results in the formation of a mixture of three identifiable crystalline compounds, namely [Pb10{S‐2,6‐(CH3)2C6H3}20], [Pb6S{S‐2,6‐(CH3)2C6H3}10(C4H8O)4] and [Pb8O2{S‐2,6‐(CH3)2C6H3}12]. In contrast, fractional crystallization from dilute solutions initially yielded only yellow crystals of [Pb14O6{S‐2,6‐(CH3)2C6H3}16]. Further concentration of the supernatant solution yielded, upon layering with pentane, [Pb6S{S‐2,6‐(CH3)2C6H3}10(C4H8O)4] and [Pb10{S‐2,6‐(CH3)2C6H3}20], which are almost completely separable by controlling the duration of the crystallization step and the amount of condensed pentane. Recrystallization of the crude orange powder under aerobic conditions produces pure [Pb14O6{S‐2,6‐(CH3)2C6H3}16] with a yield five times higher than that under nitrogen. This shows that it is sensitive to oxidation by oxygen in solution. The structures of all four complexes have been determined by single‐crystal X‐ray analysis. The net formed by the six oxygen and twelve lead atoms in the center of [Pb14O6{S‐2,6‐(CH3)2C6H3}16] resembles a small piece of a layer of the solid‐state structure of red PbO. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005)

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Metal (Li, Ge^II, Ge^III, Sn^II, and Pb^II) 2,6-dialkylbenzenethiolates; X-ray crystal structures of Sn(SAr)₂(Ar = C₆H₂Bu^t₃-2,4,6) and [M(SAr′)₂]³(M = Sn or Pb, Ar′= C₆H₃Prⁱ₂-2,6)

Cited by 74 publications

References 0 publications

Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se

Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se

Dispersion Forces and Counterintuitive Steric Effects in Main Group Molecules: Heavier Group 14 (Si–Pb) Dichalcogenolate Carbene Analogues with Sub-90° Interligand Bond Angles

Four New Lead(II) Thiolate Cluster Complexes – Unexpected Products of a Conventional Synthesis

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Metal (Li, GeII, GeIII, SnII, and PbII) 2,6-dialkylbenzenethiolates; X-ray crystal structures of Sn(SAr)2(Ar = C6H2But3-2,4,6) and [M(SAr′)2]3(M = Sn or Pb, Ar′= C6H3Pri2-2,6)

Cited by 74 publications

References 0 publications

Syntheses and X-ray structural analyses of [(C6H5)4As][Sn(EC6H5)3], E = S and Se

Syntheses and X-ray structural analyses of [(C6H5)4As][Sn(EC6H5)3], E = S and Se

Dispersion Forces and Counterintuitive Steric Effects in Main Group Molecules: Heavier Group 14 (Si–Pb) Dichalcogenolate Carbene Analogues with Sub-90° Interligand Bond Angles

Four New Lead(II) Thiolate Cluster Complexes – Unexpected Products of a Conventional Synthesis

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Metal (Li, Ge^II, Ge^III, Sn^II, and Pb^II) 2,6-dialkylbenzenethiolates; X-ray crystal structures of Sn(SAr)₂(Ar = C₆H₂Bu^t₃-2,4,6) and [M(SAr′)₂]³(M = Sn or Pb, Ar′= C₆H₃Prⁱ₂-2,6)

Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se

Syntheses and X-ray structural analyses of [(C₆H₅)₄As][Sn(EC₆H₅)₃], E = S and Se