Solution and Solid-State Characterization of PbSe Precursors

Prathamesh B. Vartak; Zhongyong Wang; Thomas L. Groy; Ryan J. Trovitch; Robert Y. Wang

doi:10.1021/acsomega.9b03715

Solution and Solid-State Characterization of PbSe Precursors

Prathamesh B. Vartak, Zhongyong Wang, Thomas L. Groy, Ryan J. Trovitch, Robert Y. Wang

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Abstract

The addition of lead to diphenyl diselenide in ethylenediamine (en) or pyridine (py) allowed for the observation of the solvento complexes, (en)Pb(SePh)₂ or (py)₂Pb(SePh)₂, respectively. Performing this reaction in dimethyl sulfoxide and subsequent crystallization was found to afford Pb(SePh)₂. Inductively coupled plasma optical emission spectroscopy revealed a 1:2 lead to selenium ratio for all three complexes. Nuclear magnetic resonance spectroscopy confirms that Pb(SePh)₂ is readily solubilized by ethylenediamine, and electrospray ionization mass spectrometry supports the presence of Pb(SePh)₂ moieties in solution. Single-crystal X-ray diffraction analysis of the pyridine adduct, (py)₂Pb(SePh)₂, revealed a seesaw molecular geometry featuring equatorial phenylselenolate ligands. Crystals of Pb(SePh)₂ grown from dimethyl sulfoxide revealed one-dimensional polymeric chains of Pb(SePh)₂. We believe that the lead(II) phenylselenolate complexes form via an oxidative addition reaction.

Original language	English (US)
Pages (from-to)	1949-1955
Number of pages	7
Journal	ACS Omega
Volume	5
Issue number	4
DOIs	https://doi.org/10.1021/acsomega.9b03715
State	Published - Feb 4 2020

ASJC Scopus subject areas

General Chemistry
General Chemical Engineering

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10.1021/acsomega.9b03715

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@article{060656874a5e44649cefa28a63c3a753,

title = "Solution and Solid-State Characterization of PbSe Precursors",

abstract = "The addition of lead to diphenyl diselenide in ethylenediamine (en) or pyridine (py) allowed for the observation of the solvento complexes, (en)Pb(SePh)2 or (py)2Pb(SePh)2, respectively. Performing this reaction in dimethyl sulfoxide and subsequent crystallization was found to afford Pb(SePh)2. Inductively coupled plasma optical emission spectroscopy revealed a 1:2 lead to selenium ratio for all three complexes. Nuclear magnetic resonance spectroscopy confirms that Pb(SePh)2 is readily solubilized by ethylenediamine, and electrospray ionization mass spectrometry supports the presence of Pb(SePh)2 moieties in solution. Single-crystal X-ray diffraction analysis of the pyridine adduct, (py)2Pb(SePh)2, revealed a seesaw molecular geometry featuring equatorial phenylselenolate ligands. Crystals of Pb(SePh)2 grown from dimethyl sulfoxide revealed one-dimensional polymeric chains of Pb(SePh)2. We believe that the lead(II) phenylselenolate complexes form via an oxidative addition reaction.",

author = "Vartak, {Prathamesh B.} and Zhongyong Wang and Groy, {Thomas L.} and Trovitch, {Ryan J.} and Wang, {Robert Y.}",

note = "Publisher Copyright: {\textcopyright} 2020 American Chemical Society.",

year = "2020",

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day = "4",

doi = "10.1021/acsomega.9b03715",

language = "English (US)",

volume = "5",

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journal = "ACS Omega",

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T1 - Solution and Solid-State Characterization of PbSe Precursors

AU - Vartak, Prathamesh B.

AU - Wang, Zhongyong

AU - Groy, Thomas L.

AU - Trovitch, Ryan J.

AU - Wang, Robert Y.

PY - 2020/2/4

Y1 - 2020/2/4

N2 - The addition of lead to diphenyl diselenide in ethylenediamine (en) or pyridine (py) allowed for the observation of the solvento complexes, (en)Pb(SePh)2 or (py)2Pb(SePh)2, respectively. Performing this reaction in dimethyl sulfoxide and subsequent crystallization was found to afford Pb(SePh)2. Inductively coupled plasma optical emission spectroscopy revealed a 1:2 lead to selenium ratio for all three complexes. Nuclear magnetic resonance spectroscopy confirms that Pb(SePh)2 is readily solubilized by ethylenediamine, and electrospray ionization mass spectrometry supports the presence of Pb(SePh)2 moieties in solution. Single-crystal X-ray diffraction analysis of the pyridine adduct, (py)2Pb(SePh)2, revealed a seesaw molecular geometry featuring equatorial phenylselenolate ligands. Crystals of Pb(SePh)2 grown from dimethyl sulfoxide revealed one-dimensional polymeric chains of Pb(SePh)2. We believe that the lead(II) phenylselenolate complexes form via an oxidative addition reaction.

AB - The addition of lead to diphenyl diselenide in ethylenediamine (en) or pyridine (py) allowed for the observation of the solvento complexes, (en)Pb(SePh)2 or (py)2Pb(SePh)2, respectively. Performing this reaction in dimethyl sulfoxide and subsequent crystallization was found to afford Pb(SePh)2. Inductively coupled plasma optical emission spectroscopy revealed a 1:2 lead to selenium ratio for all three complexes. Nuclear magnetic resonance spectroscopy confirms that Pb(SePh)2 is readily solubilized by ethylenediamine, and electrospray ionization mass spectrometry supports the presence of Pb(SePh)2 moieties in solution. Single-crystal X-ray diffraction analysis of the pyridine adduct, (py)2Pb(SePh)2, revealed a seesaw molecular geometry featuring equatorial phenylselenolate ligands. Crystals of Pb(SePh)2 grown from dimethyl sulfoxide revealed one-dimensional polymeric chains of Pb(SePh)2. We believe that the lead(II) phenylselenolate complexes form via an oxidative addition reaction.

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U2 - 10.1021/acsomega.9b03715

DO - 10.1021/acsomega.9b03715

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SN - 2470-1343

VL - 5

SP - 1949

EP - 1955

JO - ACS Omega

JF - ACS Omega

IS - 4

ER -

Solution and Solid-State Characterization of PbSe Precursors

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CCDC 1955117: Experimental Crystal Structure Determination

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Solution and Solid-State Characterization of PbSe Precursors

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CCDC 1955117: Experimental Crystal Structure Determination

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