A new pathway to Mg2Ni and an MgNi carbide

Organometallic Access to Intermetallic θ‐CuE2 (E = Al, Ga) and Cu1–xAlx Phases

“…[ [35] The solid-state 27 Al MAS NMR spectrum (see Supporting Information) exhibits a Knight shift at δ = 1640 ppm, which is assignable to Al 0 and in agreement with our previous work by using [(AlCp*) 4 ] as a precursor [22a] and the data of Al powder reported in the literature. [36] Two signals for Al 2 O 3 are observed at δ = 56 and 1 ppm, depending on the nature of the coordination geometry of the AlO x species.…”

“…Further, a weak signal of H 2 at δ = 4.61 ppm is observed. The 27 Al NMR spectrum evidences the disappearance of the starting material. In addition, no Al-containing species are noted, which is indicative of quantitative decomposition of [(Me 3 N)AlH 3 ].…”

“…The 1 H NMR spectrum of the precursor [(Me 3 N)AlH 3 ] shows a broad signal at δ = 3.81 ppm, which is assignable to the Al-H atoms, and a sharp singlet at δ = 1.93 ppm for the hydrogen atoms of the coordinated NMe 3 molecule. The corresponding 27 Al NMR spectrum exhibits a broad resonance at δ = 136 ppm for the starting material. The 1 H NMR spectrum recorded after treatment with 3 bar H 2 at 150°C for 24 h does not exhibit the hydride signals, whereas the signal for the NMe 3 moiety shifts to 2.10 ppm (free amine).…”

“…Accordingly, in the 31 P NMR spectrum, only the signal of PMe 3 was found at δ = -62.2 ppm. The 27 Al NMR spectrum did not exhibit any signals. The X-ray diffractogram (Figure 4a) of the isolated powder as described above clearly exhibits the characteristic reflections of the θ-CuAl 2 phase (body-centered tetragonal I4/mcm, JCPDS No.…”

“…Buhro et al showed that this compound decomposes to Al 0 by thermolysis in organic solution with the gaseous byproducts H 2 and NMe 3 . [26] It is well established that metal hydrides and anionic hydride complexes, such as Bogdanović's MgH 2 [27] or LiAlH 4 , [28][29][30] serve as precursors for the precursor synthesis of metal alloys. Accordingly, we recently showed that [(Me 3 N)AlH 3 ] and [Ni(cod) 2 ] (cod = cis,cis-1,5-cyclooctadiene) rapidly react to afford NiAl nanoparticles under hydrogen pressure.…”