TY - JOUR
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.
N1 - Funding Information:
This work was supported by the National Science Foundation through award number DMR-1506829.
Funding Information:
We acknowledge the use of facilities within Goldwater Environmental Laboratory, Mass Spectrometry Facility, Magnetic Resonance Research Center, and the Eyring Materials Center (supported in part by NNCI-ECCS-1542160) at Arizona State University. We also thank Brian Cherry, Daniel Brune, Megan Maurer, Jia Fan, Natasha Zolotova, and Cathy Kochert for insightful discussions.
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
M3 - Article
AN - SCOPUS:85078994475
VL - 5
SP - 1949
EP - 1955
JO - ACS Omega
JF - ACS Omega
SN - 2470-1343
IS - 4
ER -