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Loose, Florian

Publications and source records attributed to Loose, Florian.

Beyond Ammonia: Nitrogen–Element Bond Forming Reactions with Coordinated Dinitrogen

The functionalization of coordinated dinitrogen to form nitrogen-element bonds en route to nitrogen-containing molecules is a long-standing challenge in chemical synthesis. The strong triple bond and the non-polarity of the N 2 molecule pose thermodynamic and kinetic challenges for promoting reactivity. Although heterogeneous, homogeneous and biological catalysts are all known for catalytic nitrogen fixation to ammonia, the catalytic synthesis of more complicated nitrogen-containing organic molecules has far less precedent. Examples of silyl radical additions to coordinated nitrogen to form silylamines stands as the lone example of a catalytic reaction involving N 2 to form a product other than ammonia. Our review surveys the field of molecular transition metal complexes, as well as recent boron examples for the formation of nitrogen-element bonds. Emphasis is placed on the coordination and activation modes of N 2 in the various metal compounds from across the transition series and how these structures can rationally inform reactivity studies. Over the past few decades, the field has evolved from the addition of carbon electrophiles in a manner similar to protonation reactions to more organometallic-inspired reactivity including insertions, 1,2-additions and cycloadditions. Various N–C, N–Si and N–B bond-forming reactions have been discovered highlighting that the challenge for catalytic chemistry is not in the reactivity of coordinated dinitrogen but rather removal of the functionalized ligand from the coordination sphere of the metal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Catalytic Hydrogenation of a Manganese(V) Nitride to Ammonia

The catalytic hydrogenation of a metal nitride to make free ammonia using a rhodium hydride catalyst that promotes H 2 activation and hydrogen atom transfer is described. The phenylimine-substituted rhodium complex, (η 5 -C 5 Me 5 )Rh( Me PhI)H ( Me PhI = N-methyl-1-phenylethan-1-imine) exhibited higher thermal stability compared to the previously reported (η 5 -C 5 Me 5 )Rh(ppy)H (ppy = 2-phenylpyridine). DFT calculations established that the two rhodium complexes have comparable Rh–H bond dissociation free energies of 51.8 kcal mol-1 for (η 5 -C 5 Me 5 )Rh(MePhI)H and 51.1 kcal mol -1 for (η 5 -C 5 Me 5 )Rh(ppy)H. In the presence of 10 mol% of the phe-nylimine rhodium precatalyst and 4 atm of H 2 in THF, the manganese nitride, ( tBu Salen)Mn≡N underwent hydrogenation to liberate free ammonia with up to 6 total turnovers of NH 3 or 18 turnovers of H·. The phenylpyridine analogue proved inactive for ammonia synthesis under identical conditions owing to competing deleterious hydride transfer chemistry. Subsequent research showed that the use of a non-polar solvent such as benzene suppressed formation of the cationic rhodium product resulting from the hydride transfer and enabled catalytic ammonia synthesis by proton coupled electron transfer.

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