Kurogi, Takashi; Chu, Jiaxiang; Chen, Yaofeng; Mindiola, Daniel J. published an article in 2019, the title of the article was Neutral and Anionic Monomeric Zirconium Imides Prepared via Selective C=N Bond Cleavage of a Multidentate and Sterically Demanding β-Diketiminato Ligand.HPLC of Formula: 574-98-1 And the article contains the following content:
A sterically encumbering multidentate β-diketiminato ligand, tBuL2 (tBuL2=[ArNC(tBu)CHC(tBu)NCH2CH2N(Me)CH2CH2NMe2]-, Ar = 2,6-iPr2C6H3), is reported in this study along with its coordination chem. to zirconium(IV). Using the lithio salt of this ligand, Li(tBuL2) (4), the zirconium(IV) precursor (tBuL2)ZrCl3 (6) could be readily prepared in 85% yield and structurally characterized. Reduction of 6 with 2 equiv of KC8 gave the terminal and mononuclear zirconium imide-chloride [C(tBu)CHC(tBu)NCH2CH2N(Me)CH2CH2NMe2]Zr(=NAr)(Cl) (7) as the result of reductive C=N cleavage of the imino fragment in the multidentate ligand tBuL2 by an elusive ZrII species (tBuL2)ZrCl (A). The azabutadienyl ligand in 7 can be further reduced by 2 e- with KC8 to afford the anionic imide [K(THF)2]{[CH(tBu)CHC(tBu)NCH2CH2N(Me)CH2CH2N(Me)CH2]Zr = NAr} (8-2THF) in 42% isolated yield. Complex 8-2THF results from the oxidative addition of an amine C-H bond followed by migration to the vinylic group of the formal [C(tBu)CHC(tBu)NCH2CH2N(Me)CH2CH2NMe2]- ligand in 7. All halides in 6 can be replaced with azides to afford (tBuL2)Zr(N3)3 (9) which was structurally characterized, and reduction with two equiv of KC8 also results in C=N bond cleavage of tBuL2 to form [C(tBu)CHC(tBu)NCH2CH2N(Me)CH2CH2NMe2]Zr(=NAr)(N3) (10), instead of the expected azide disproportionation to N3- and N2. Solid-state single crystal structural studies confirm the formation of mononuclear and terminal zirconium imido groups in 7, 8-Et2O, and 10 with Zr = NAr distances being 1.8776(10), 1.9505(15), and 1.881(3) Å, resp. The experimental process involved the reaction of 2-(2-Bromoethyl)isoindoline-1,3-dione(cas: 574-98-1).HPLC of Formula: 574-98-1
The Article related to zirconium lithium diketiminato azide complex preparation crystal structure, azides, imides, reduction, zirconium, Inorganic Chemicals and Reactions: Coordination Compounds and other aspects.HPLC of Formula: 574-98-1
Referemce:
Bromide – Wikipedia,
bromide – Wiktionary