Tribasic lead maleate and lead maleate: Synthesis and structural and spectroscopic characterizations

François Bonhomme; Todd M. Alam; Aaron J. Celestian; David R. Tallant; Timothy J. Boyle; Brian R. Cherry; Ralph G. Tissot; Mark A. Rodriguez; John B. Parise; May Nyman

doi:10.1021/ic050611y

Tribasic lead maleate and lead maleate: Synthesis and structural and spectroscopic characterizations

François Bonhomme, Todd M. Alam, Aaron J. Celestian, David R. Tallant, Timothy J. Boyle, Brian R. Cherry, Ralph G. Tissot, Mark A. Rodriguez, John B. Parise, May Nyman

Arizona State University

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

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Abstract

We report on the synthesis and structure of tribasic lead maleate hemihydrate ([Pb₄O₃]C₂H₂(CO ₂)₂·1/2H₂O, TRIMAL) and lead maleate (PbC₂H₂(CO₂)₂, PBMAL). The structure of [Pb₄O₃]C₂H₂(CO₂) ₂·1/2H₂O, solved ab initio from X-ray powder diffraction data, consists of infinite slabs of edge-sharing OPb₄ tetrahedra, of composition [Pb₄O₃], running along the c axis and linked together into a three-dimensional network by tetradentate maleate anionic ligands. The structure of PbC₂H₂(CO ₂)₂, solved from single crystal diffraction data, is lamellar and contains double layers of heptacoordinated lead atoms, bonded only to the oxygen atoms of the maleate ligands. In both compounds, lead is in the oxidation state 2+ and the coordination polyhedra around the Pb²⁺ exhibit a hemidirected geometry and are strongly distorted as a result of the lone pair of electrons. The absence of protons on the acidic portion of the maleate moieties was confirmed by Raman spectroscopy and by ¹H MAS and ¹H-¹³C CP MAS NMR experiments. The two compounds were further characterized using chemical and thermogravimetric analyses.

Original language	English (US)
Pages (from-to)	7394-7402
Number of pages	9
Journal	Inorganic chemistry
Volume	44
Issue number	21
DOIs	https://doi.org/10.1021/ic050611y
State	Published - Oct 17 2005

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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title = "Tribasic lead maleate and lead maleate: Synthesis and structural and spectroscopic characterizations",

abstract = "We report on the synthesis and structure of tribasic lead maleate hemihydrate ([Pb4O3]C2H2(CO 2)2·1/2H2O, TRIMAL) and lead maleate (PbC2H2(CO2)2, PBMAL). The structure of [Pb4O3]C2H2(CO2) 2·1/2H2O, solved ab initio from X-ray powder diffraction data, consists of infinite slabs of edge-sharing OPb4 tetrahedra, of composition [Pb4O3], running along the c axis and linked together into a three-dimensional network by tetradentate maleate anionic ligands. The structure of PbC2H2(CO 2)2, solved from single crystal diffraction data, is lamellar and contains double layers of heptacoordinated lead atoms, bonded only to the oxygen atoms of the maleate ligands. In both compounds, lead is in the oxidation state 2+ and the coordination polyhedra around the Pb2+ exhibit a hemidirected geometry and are strongly distorted as a result of the lone pair of electrons. The absence of protons on the acidic portion of the maleate moieties was confirmed by Raman spectroscopy and by 1H MAS and 1H-13C CP MAS NMR experiments. The two compounds were further characterized using chemical and thermogravimetric analyses.",

author = "Fran{\c c}ois Bonhomme and Alam, {Todd M.} and Celestian, {Aaron J.} and Tallant, {David R.} and Boyle, {Timothy J.} and Cherry, {Brian R.} and Tissot, {Ralph G.} and Rodriguez, {Mark A.} and Parise, {John B.} and May Nyman",

year = "2005",

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T2 - Synthesis and structural and spectroscopic characterizations

AU - Bonhomme, François

AU - Alam, Todd M.

AU - Celestian, Aaron J.

AU - Tallant, David R.

AU - Boyle, Timothy J.

AU - Cherry, Brian R.

AU - Tissot, Ralph G.

AU - Rodriguez, Mark A.

AU - Parise, John B.

AU - Nyman, May

PY - 2005/10/17

Y1 - 2005/10/17

N2 - We report on the synthesis and structure of tribasic lead maleate hemihydrate ([Pb4O3]C2H2(CO 2)2·1/2H2O, TRIMAL) and lead maleate (PbC2H2(CO2)2, PBMAL). The structure of [Pb4O3]C2H2(CO2) 2·1/2H2O, solved ab initio from X-ray powder diffraction data, consists of infinite slabs of edge-sharing OPb4 tetrahedra, of composition [Pb4O3], running along the c axis and linked together into a three-dimensional network by tetradentate maleate anionic ligands. The structure of PbC2H2(CO 2)2, solved from single crystal diffraction data, is lamellar and contains double layers of heptacoordinated lead atoms, bonded only to the oxygen atoms of the maleate ligands. In both compounds, lead is in the oxidation state 2+ and the coordination polyhedra around the Pb2+ exhibit a hemidirected geometry and are strongly distorted as a result of the lone pair of electrons. The absence of protons on the acidic portion of the maleate moieties was confirmed by Raman spectroscopy and by 1H MAS and 1H-13C CP MAS NMR experiments. The two compounds were further characterized using chemical and thermogravimetric analyses.

AB - We report on the synthesis and structure of tribasic lead maleate hemihydrate ([Pb4O3]C2H2(CO 2)2·1/2H2O, TRIMAL) and lead maleate (PbC2H2(CO2)2, PBMAL). The structure of [Pb4O3]C2H2(CO2) 2·1/2H2O, solved ab initio from X-ray powder diffraction data, consists of infinite slabs of edge-sharing OPb4 tetrahedra, of composition [Pb4O3], running along the c axis and linked together into a three-dimensional network by tetradentate maleate anionic ligands. The structure of PbC2H2(CO 2)2, solved from single crystal diffraction data, is lamellar and contains double layers of heptacoordinated lead atoms, bonded only to the oxygen atoms of the maleate ligands. In both compounds, lead is in the oxidation state 2+ and the coordination polyhedra around the Pb2+ exhibit a hemidirected geometry and are strongly distorted as a result of the lone pair of electrons. The absence of protons on the acidic portion of the maleate moieties was confirmed by Raman spectroscopy and by 1H MAS and 1H-13C CP MAS NMR experiments. The two compounds were further characterized using chemical and thermogravimetric analyses.

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Tribasic lead maleate and lead maleate: Synthesis and structural and spectroscopic characterizations

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