Organolead(IV) polymers [(Me3Pb)4M(CN)6·nH2O] with M=Fe and Ru (0≤n≤2): Solid-state NMR and vibrational spectroscopy; Crystal structure of the dihydrates

Abdul K. Brimah; Peter Schwarz; R. D. Fischer; Nicola A. Davies; Robin K. Harris

doi:10.1016/S0022-328X(97)00202-7

Organolead(IV) polymers [(Me₃Pb)₄M(CN)₆·nH₂O] with M=Fe and Ru (0≤n≤2): Solid-state NMR and vibrational spectroscopy; Crystal structure of the dihydrates

Abdul K. Brimah, Peter Schwarz, R. D. Fischer, Nicola A. Davies, Robin K. Harris

Research output: Contribution to journal › Article › peer-review

18 Scopus citations

Abstract

From aqueous solutions of Me₃PbCl and K₄[M(CN)₆] (4:1; M=Fe or Ru), primarily the diaqua compounds [(Me₃Pb)₄M(CN)₆·2H₂O], 4a and 4b, precipitate. These turn out to be not the three-dimensional host-guest systems [{Me₃Pb(H₂O)₂}(Me₃Pb) ₃M(CN₆)], but to consist of infinite, puckered layers whose in-built -M-CN-Pb-OH₂ units are likely to form hydrogen bridges between the layers. 4a appears to be sensitive to even very modest influences (including grinding) and tends to lose the coordinated H₂O molecules partially or totally. This feature is monitored best by both infrared/Raman and CP MAS solid-state NMR spectroscopy. The strictly anhydrous species, 5a and 5b, strongly resemble their earlier-reported Me₃Sn-homologues in also displaying strongly temperature-dependent ¹³C solid-state NMR spectra, but show no ion-exchange activity. The ¹³C-, ¹⁵N- and ²⁰⁷Pb-NMR data in combination yield detailed information about crystallographic sites and intramolecular mobility ol' the Me₃Pb groups.

Original language	English
Pages (from-to)	1-12
Number of pages	12
Journal	Journal of Organometallic Chemistry
Volume	568
Issue number	1-2
DOIs	https://doi.org/10.1016/S0022-328X(97)00202-7
State	Published - 15 Oct 1998
Externally published	Yes

Keywords

Crystal structure
Cyanide
Iron
Lead
Magic-angle spinning
Polymer
Ruthenium
Solid-state NMR

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10.1016/S0022-328X(97)00202-7

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@article{8317fdbd90d8465296665bc9eb1670f9,

title = "Organolead(IV) polymers [(Me3Pb)4M(CN)6·nH2O] with M=Fe and Ru (0≤n≤2): Solid-state NMR and vibrational spectroscopy; Crystal structure of the dihydrates",

abstract = "From aqueous solutions of Me3PbCl and K4[M(CN)6] (4:1; M=Fe or Ru), primarily the diaqua compounds [(Me3Pb)4M(CN)6·2H2O], 4a and 4b, precipitate. These turn out to be not the three-dimensional host-guest systems [{Me3Pb(H2O)2}(Me3Pb) 3M(CN6)], but to consist of infinite, puckered layers whose in-built -M-CN-Pb-OH2 units are likely to form hydrogen bridges between the layers. 4a appears to be sensitive to even very modest influences (including grinding) and tends to lose the coordinated H2O molecules partially or totally. This feature is monitored best by both infrared/Raman and CP MAS solid-state NMR spectroscopy. The strictly anhydrous species, 5a and 5b, strongly resemble their earlier-reported Me3Sn-homologues in also displaying strongly temperature-dependent 13C solid-state NMR spectra, but show no ion-exchange activity. The 13C-, 15N- and 207Pb-NMR data in combination yield detailed information about crystallographic sites and intramolecular mobility ol' the Me3Pb groups.",

keywords = "Crystal structure, Cyanide, Iron, Lead, Magic-angle spinning, Polymer, Ruthenium, Solid-state NMR",

author = "Brimah, {Abdul K.} and Peter Schwarz and Fischer, {R. D.} and Davies, {Nicola A.} and Harris, {Robin K.}",

note = "Funding Information: We thank the UK Science and Engineering Research Council for access to the Varian VXR 300 spectrometer under the national solid-state NMR service arrangements. Financial support from the British Council and the DAAD (Bonn) under the ARC Programme, from Deutsche Forschungsgemeinschaft (until 1992) and from the Fonds der Chemischen Industrie is greatly appreciated. Professor U. Behrens, Dr S. Eller, Dr D.C. Apperley, K. Rechter and (the late) T.M. Soliman are thanked for helpful discussions (U.B., D.C.A.) and the delivery of single samples or spectra (S.E., K.R., T.M.S.), respectively.",

year = "1998",

month = oct,

day = "15",

doi = "10.1016/S0022-328X(97)00202-7",

language = "English",

volume = "568",

pages = "1--12",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier B.V.",

number = "1-2",

}

TY - JOUR

T1 - Organolead(IV) polymers [(Me3Pb)4M(CN)6·nH2O] with M=Fe and Ru (0≤n≤2)

T2 - Solid-state NMR and vibrational spectroscopy; Crystal structure of the dihydrates

AU - Brimah, Abdul K.

AU - Schwarz, Peter

AU - Fischer, R. D.

AU - Davies, Nicola A.

AU - Harris, Robin K.

N1 - Funding Information: We thank the UK Science and Engineering Research Council for access to the Varian VXR 300 spectrometer under the national solid-state NMR service arrangements. Financial support from the British Council and the DAAD (Bonn) under the ARC Programme, from Deutsche Forschungsgemeinschaft (until 1992) and from the Fonds der Chemischen Industrie is greatly appreciated. Professor U. Behrens, Dr S. Eller, Dr D.C. Apperley, K. Rechter and (the late) T.M. Soliman are thanked for helpful discussions (U.B., D.C.A.) and the delivery of single samples or spectra (S.E., K.R., T.M.S.), respectively.

PY - 1998/10/15

Y1 - 1998/10/15

N2 - From aqueous solutions of Me3PbCl and K4[M(CN)6] (4:1; M=Fe or Ru), primarily the diaqua compounds [(Me3Pb)4M(CN)6·2H2O], 4a and 4b, precipitate. These turn out to be not the three-dimensional host-guest systems [{Me3Pb(H2O)2}(Me3Pb) 3M(CN6)], but to consist of infinite, puckered layers whose in-built -M-CN-Pb-OH2 units are likely to form hydrogen bridges between the layers. 4a appears to be sensitive to even very modest influences (including grinding) and tends to lose the coordinated H2O molecules partially or totally. This feature is monitored best by both infrared/Raman and CP MAS solid-state NMR spectroscopy. The strictly anhydrous species, 5a and 5b, strongly resemble their earlier-reported Me3Sn-homologues in also displaying strongly temperature-dependent 13C solid-state NMR spectra, but show no ion-exchange activity. The 13C-, 15N- and 207Pb-NMR data in combination yield detailed information about crystallographic sites and intramolecular mobility ol' the Me3Pb groups.

AB - From aqueous solutions of Me3PbCl and K4[M(CN)6] (4:1; M=Fe or Ru), primarily the diaqua compounds [(Me3Pb)4M(CN)6·2H2O], 4a and 4b, precipitate. These turn out to be not the three-dimensional host-guest systems [{Me3Pb(H2O)2}(Me3Pb) 3M(CN6)], but to consist of infinite, puckered layers whose in-built -M-CN-Pb-OH2 units are likely to form hydrogen bridges between the layers. 4a appears to be sensitive to even very modest influences (including grinding) and tends to lose the coordinated H2O molecules partially or totally. This feature is monitored best by both infrared/Raman and CP MAS solid-state NMR spectroscopy. The strictly anhydrous species, 5a and 5b, strongly resemble their earlier-reported Me3Sn-homologues in also displaying strongly temperature-dependent 13C solid-state NMR spectra, but show no ion-exchange activity. The 13C-, 15N- and 207Pb-NMR data in combination yield detailed information about crystallographic sites and intramolecular mobility ol' the Me3Pb groups.

KW - Crystal structure

KW - Cyanide

KW - Iron

KW - Lead

KW - Magic-angle spinning

KW - Polymer

KW - Ruthenium

KW - Solid-state NMR

UR - http://www.scopus.com/inward/record.url?scp=0002737791&partnerID=8YFLogxK

U2 - 10.1016/S0022-328X(97)00202-7

DO - 10.1016/S0022-328X(97)00202-7

M3 - Article

AN - SCOPUS:0002737791

SN - 0022-328X

VL - 568

SP - 1

EP - 12

JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

IS - 1-2

ER -

Organolead(IV) polymers [(Me₃Pb)₄M(CN)₆·nH₂O] with M=Fe and Ru (0≤n≤2): Solid-state NMR and vibrational spectroscopy; Crystal structure of the dihydrates

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