Synthesis and structure of (Ph4P)2MCl6 (M = Ti, Zr, Hf, Th, U, Np, Pu)

Inorganic Chemistry
Stefan G MinasianDavid K Shuh

Abstract

High-purity syntheses are reported for a series of first, second, and third row transition metal and actinide hexahalide compounds with equivalent, noncoordinating countercations: (Ph(4)P)(2)TiF(6) (1) and (Ph(4)P)(2)MCl(6) (M = Ti, Zr, Hf, Th, U, Np, Pu; 2-8). While a reaction between MCl(4) (M = Zr, Hf, U) and 2 equiv of Ph(4)PCl provided 3, 4, and 6, syntheses for 1, 2, 5, 7, and 8 required multistep procedures. For example, a cation exchange reaction with Ph(4)PCl and (NH(4))(2)TiF(6) produced 1, which was used in a subsequent anion exchange reaction with Me(3)SiCl to synthesize 2. For 5, 7, and 8, synthetic routes starting with aqueous actinide precursors were developed that circumvented any need for anhydrous Th, Np, or Pu starting materials. The solid-state geometries, bond distances and angles for isolated ThCl(6)(2-), NpCl(6)(2-), and PuCl(6)(2-) anions with noncoordinating counter cations were determined for the first time in the X-ray crystal structures of 5, 7, and 8. Solution phase and solid-state diffuse reflectance spectra were also used to characterize 7 and 8. Transition metal MCl(6)(2-) anions showed the anticipated increase in M-Cl bond distances when changing from M = Ti to Zr, and then a decrease from Zr to...Continue Reading

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Citations

Nov 8, 2012·Chemical Reviews·Matthew B Jones, Andrew J Gaunt
Aug 1, 2015·Inorganic Chemistry·Richard E Wilson
Jul 22, 2016·Nature Chemistry·Michał S DutkiewiczPolly L Arnold
Jun 15, 2017·Journal of the American Chemical Society·Justin N CrossPing Yang
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Jan 9, 2020·Chemistry : a European Journal·Korey P CarterRebecca J Abergel
Sep 10, 2020·Chemistry : a European Journal·Thomas RadoskeThorsten Stumpf
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Mar 2, 2018·Inorganic Chemistry·David D Schnaars, Richard E Wilson
May 24, 2019·Journal of the American Chemical Society·Thibault CheissonEric J Schelter
Oct 9, 2020·Inorganic Chemistry·Roger KloditzJuliane März
Aug 2, 2017·Inorganic Chemistry·Jennifer N WackerKarah E Knope
Jul 30, 2019·Inorganic Chemistry·Jennifer N WackerKarah E Knope
Jul 13, 2019·Inorganic Chemistry·Jennifer N WackerKarah E Knope
Dec 13, 2018·Journal of the American Chemical Society·Jing SuPing Yang

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