Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.

Pagano, Justin Kane; Scott, Brian Lindley; Kiplinger, Jaqueline Loetsch

doi:10.1016/j.ica.2018.06.010

Title: Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.

Abstract

Two new uranium metallacyclopropenes, (C₅Me₄R)₂U(η²-Ph₂PC=CPPh₂) (R = Me, Et) were prepared by reducing the corresponding (C₅Me₄R)₂UCl₂ complexes with KC₈ in the presence of 1,2-bis(diphenylphosphino)acetylene (Ph₂P–C≡C–PPh₂). Both compounds were fully characterized by a combination of elemental analysis and multinuclear NMR, UV–visible–NIR, and IR spectroscopies. Differences in the electronic spectra of these novel compounds and the known (C₅Me₅)₂U(η²-Me₃SiC=CSiMe₃) are discussed. Finally, also presented is the solid-state structure of (C₅Me₄Et)₂U(η²-Ph₂PC=CPPh₂), which reveals significant distortions of the coordinated 1,2-bis(diphenylphosphino)acetylene (Ph₂P–C≡C–PPh₂) ligand.

Authors:

^[1];

^[1]

Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Publication Date:: Sat Jun 09 00:00:00 EDT 2018

Research Org.:: Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Sponsoring Org.:: USDOE National Nuclear Security Administration (NNSA); USDOE Laboratory Directed Research and Development (LDRD) Program

OSTI Identifier:: 1454999

Alternate Identifier(s):: OSTI ID: 1601299

Report Number(s):: LA-UR-17-31363
Journal ID: ISSN 0020-1693; TRN: US1901188

Grant/Contract Number:: AC52-06NA25396

Resource Type:: Accepted Manuscript

Journal Name:: Inorganica Chimica Acta

Additional Journal Information:: Journal Volume: 482; Journal ID: ISSN 0020-1693

Publisher:: Elsevier

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Uranium; Phosphorous; Metallacyclopropene; Electronic Spectroscopy; X-ray Crystallography

Citation Formats


                    Pagano, Justin Kane, Scott, Brian Lindley, and Kiplinger, Jaqueline Loetsch. Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes..  United States: N. p., 2018. 
Web.  doi:10.1016/j.ica.2018.06.010.

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                    Pagano, Justin Kane, Scott, Brian Lindley, & Kiplinger, Jaqueline Loetsch. Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes..  United States.  https://doi.org/10.1016/j.ica.2018.06.010

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                    Pagano, Justin Kane, Scott, Brian Lindley, and Kiplinger, Jaqueline Loetsch. Sat .  
"Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.".  United States.  https://doi.org/10.1016/j.ica.2018.06.010.  https://www.osti.gov/servlets/purl/1454999.

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@article{osti_1454999,

  title        = {Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.},

  author       = {Pagano, Justin Kane and Scott, Brian Lindley and Kiplinger, Jaqueline Loetsch},

  abstractNote = {Two new uranium metallacyclopropenes, (C5Me4R)2U(η2-Ph2PC=CPPh2) (R = Me, Et) were prepared by reducing the corresponding (C5Me4R)2UCl2 complexes with KC8 in the presence of 1,2-bis(diphenylphosphino)acetylene (Ph2P–C≡C–PPh2). Both compounds were fully characterized by a combination of elemental analysis and multinuclear NMR, UV–visible–NIR, and IR spectroscopies. Differences in the electronic spectra of these novel compounds and the known (C5Me5)2U(η2-Me3SiC=CSiMe3) are discussed. Finally, also presented is the solid-state structure of (C5Me4Et)2U(η2-Ph2PC=CPPh2), which reveals significant distortions of the coordinated 1,2-bis(diphenylphosphino)acetylene (Ph2P–C≡C–PPh2) ligand.},

  doi          = {10.1016/j.ica.2018.06.010},

  journal      = {Inorganica Chimica Acta},

  number       = ,

  volume       = 482,

  place        = {United States},

  year         = {Sat Jun 09 00:00:00 EDT 2018},

  month        = {Sat Jun 09 00:00:00 EDT 2018}

}

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Figure 1: Molecular structure of (C₅Me₄Et)₂U(η²-Ph₂PC=CPPh₂) (5) (left) and front-on view (right) showing distortions of the coordinated 1,2-bis(diphenylphosphino)acetylene ligand. Hydrogen atoms and an Et₂O solvent molecule were omitted for clarity in both images; phenyl carbons were removed for clarity in the front-on view. Thermal ellipsoids are displayed at the 50%more »

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Works referenced in this record:

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Title: Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.

Abstract

Citation Formats

Figures / Tables:

Synthesis and characterization of a new and electronically unusual uranium metallacyclocumulene, (C5Me5)2U(η4-1,2,3,4-PhC4Ph) journal, February 2017

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