<i>catena</i>-Poly[[bis(pyridine)lead(II)]bis(μ-pentafluorobenzenethiolato)]

Appleton, Sarah E.; Briand, Glen G.; Decken, Andreas; Smith, Anita S.

doi:10.1107/s160053681101659x

Cited by 5 publications

(3 citation statements)

References 7 publications

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“…The structures of 3 and 4 (Figure a) contain stacks of M(II) atoms that are formally bound to two pyridine and two selenolate ligands and datively bound to the two selenolate ligands bonded to the M(II) atom related to the first by simple translation along the b -axis, thus forming an infinite array of octahedrally arranged ligands with two M–Se bonds of ∼2.7 Å, typical lengths of such bonds in M(II) compounds, , and two dative M-Se interactions spanning ∼3.7 Å; the same structure was communicated in the structure report of Pb(SeC 6 F 5 ) 2 . For comparison, the solid-state structure of SnSe is a distorted NaCl lattice with three short (2.77, 2.82, and 2.82 Å) and three long (3.35, 3.35, and 3.47 Å) Sn–Se separations .…”

Section: Resultsmentioning

confidence: 99%

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

et al. 2015

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Reductive cleavage of C6F5SeSeC6F5 with elemental M (M = Cu, In, Sn, Pb) in pyridine results in the formation of (py)4Cu2(SeC6F5)2, (py)2In(SeC6F5)3, (py)2Sn(SeC6F5)2, and (py)2Pb(SeC6F5)2. Each group adopts a unique structure: the Cu(I) compound crystallizes as a dimer with a pair of bridging selenolates, two pyridine ligands coordinating to each Cu(I) ion, and a short Cu(I)-Cu(I) distance (2.595 Å). The indium compound crystallizes as monometallic five-coordinate (py)2In(SeC6F5)3 in a geometry that approximates a trigonal bipyramidal structure with two axial pyridine ligands and three selenolates. The tin and lead derivatives (py)2M(SeC6F5)2 are also monomeric, but they adopt nearly octahedral geometries with trans pyridine ligands, a pair of cis-selenolates, and two "empty" cis-positions on the octahedron that are oriented toward extremely remote selenolates (M-Se = 3.79 Å (Sn), 3.70 Å (Pb)) from adjacent molecules. Two of the four compounds (Cu, In) exhibit intermolecular π-π stacking arrangements in the solid state, whereas the stacking of molecules for the other two compounds (Sn, Pb) appears to be based upon molecular shape and crystal packing forces. All compounds are volatile and decompose at elevated temperatures to give MSex and Se(C6F5)2.The electronic structures of the dimeric Cu compound and monomeric (py)2M(SeC6F5)2 (M = Sn, Pb) were examined with density functional theory calculations.

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Section: Resultsmentioning

confidence: 99%

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

et al. 2015

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“…11,[13][14][15][16] The preference for high coordination numbers typically manifests itself in the formation of polymeric species, as is observed in the solid-state structures of the Pb(II) thiolates [(RS) 2 Pb] 4 (R = C 6 H 5 , 4-MeC 6 H 4 , CH 2 ) [17][18][19][20] via extensive intermolecular Pb⋯S interactions. [21][22][23][24] Unfortunately, this results in inherent insolubility in these compounds, 25 which has delayed the development of their structural chemistry.…”

Section: Introductionmentioning

confidence: 99%

Structural variation in ethylenediamine and -diphosphine adducts of (2,6-Me2C6H3S)2Pb: a single crystal X-ray diffraction and 207Pb solid-state NMR spectroscopy study

et al. 2013

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Coordination complexes of (2,6-Me2C6H3S)2Pb (1) with flexible bidentate ligands have been prepared to explore new bonding environments for Pb(II) thiolates. The reaction of 1 with a series of ethylenediamine and ethylenediphosphine ligands resulted in isolation of the adducts [(2,6-Me2C6H3S)2Pb]2(tmeda) (9), [(2,6-Me2C6H3S)2Pb]3(dmpe) (10) and [(2,6-Me2C6H3S)2Pb]2(dppe) (11) [tmeda = N,N,N',N'-tetramethylethylenediamine; dmpe = bis(dimethylphosphino)ethane; dppe = bis(diphenylphosphino)ethane]. The X-ray crystal structure of 9 shows a dinuclear species in which tmeda is chelating a ψ-trigonal bipyramidal S2N2 Pb centre via axial and equatorial sites. The structure of 10 displays a trinuclear structural unit in which dmpe is chelating a ψ-trigonal bipyramidal S2P2 Pb centre via equatorial sites. Compounds 9 and 10 also contain a second unique metal centre with ψ-tetrahedral S3Pb bonding motifs. The structure of 11 shows the dppe ligand bridging two Pb ψ-tetrahedral S2P metal bonding environments. Static (207)Pb solid-state NMR (SSNMR) spectra of 9-11 and [Ph4As][(PhS)3Pb] (12) were acquired with cross polarization (CP)-CPMG and frequency swept pulse (WURST)-CPMG pulse sequences, and the efficiencies of these pulse sequences are compared. The (207)Pb SSNMR spectra reveal that the lead chemical shift anisotropies (CSA) vary greatly between the different Pb sites, and are generally large in magnitude. DFT calculations are utilized to relate the orientations of the (207)Pb nuclear magnetic shielding tensors to the molecular structures, and to aid in spectral assignment where multiple Pb centres are present. The combination of X-ray diffraction, (207)Pb SSNMR and DFT is shown to be invaluable for the structural characterization of these important structural motifs, and should find wide-ranging application to numerous lead coordination compounds.

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“…2). Such contacts are common for indium and other heavy main group metal chalcogenolates due to their large metal radii and potential for high coordination numbers (Briand et al, 2010(Briand et al, , 2011(Briand et al, , 2012Appleton et al, 2011). This leads to the formation of insoluble materials for iBuIn(SPh) 2 (Nomura et al, 1989).…”

Section: Supramolecular Featuresmentioning

confidence: 99%

Synthesis and crystal structure of bis(μ-2-methylbenzenethiolato-κ²S:S)bis[methyl(2-methylbenzenethiolato-κS)indium(III)]

et al. 2017

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catena-Poly[[bis(pyridine)lead(II)]bis(μ-pentafluorobenzenethiolato)]

Cited by 5 publications

References 7 publications

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

Structural variation in ethylenediamine and -diphosphine adducts of (2,6-Me2C6H3S)2Pb: a single crystal X-ray diffraction and 207Pb solid-state NMR spectroscopy study

Synthesis and crystal structure of bis(μ-2-methylbenzenethiolato-κ²S:S)bis[methyl(2-methylbenzenethiolato-κS)indium(III)]

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catena-Poly[[bis(pyridine)lead(II)]bis(μ-pentafluorobenzenethiolato)]

Cited by 5 publications

References 7 publications

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSex

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSex

Structural variation in ethylenediamine and -diphosphine adducts of (2,6-Me2C6H3S)2Pb: a single crystal X-ray diffraction and 207Pb solid-state NMR spectroscopy study

Synthesis and crystal structure of bis(μ-2-methylbenzenethiolato-κ2S:S)bis[methyl(2-methylbenzenethiolato-κS)indium(III)]

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Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

Copper, Indium, Tin, and Lead Complexes with Fluorinated Selenolate Ligands: Precursors to MSe_x

Synthesis and crystal structure of bis(μ-2-methylbenzenethiolato-κ²S:S)bis[methyl(2-methylbenzenethiolato-κS)indium(III)]