1445-79-0Relevant academic research and scientific papers
The Synthesis and Properties of Dimethylgallane: Structure of the Dimer Me2Ga(μ-H)2GaMe2 in the Gas Phase as determined by Electron Diffraction
Baxter, Paul L.,Downs, Anthony J.,Goode, Michael J.,Rankin, David W. H.,Robertson, Heather E.
, p. 805 - 806 (1986)
Dimethylgallane, best synthesised by the reaction between trimethylgallane and sodium tetrahydrogallate, has been characterised by its spectroscopic and chemical properties; electron diffraction has established the structure of the dimer Me2Ga(μ-H)2GaMe2,
"Metastable" Lu(GaMe4)3 reacts like masked [LuMe3]: Synthesis of an unsolvated lanthanide dimethyl complex
Zimmermann, Melanie,Litlabo, Rannveig,Toernroos, Karl W.,Anwander, Reiner
, p. 6646 - 6649 (2009)
Homoleptic tetramethylgallate Lu(GaMe4)3 reacts selectively with superbulky (TptBu,Me)H according to a methane elimination reaction, affording the quantitative formation of monomeric base-free low-coordinate (Tp
Coordination complexes derived from 3,6-di(2-pyridyl)-1,4-dihydro-1,2,4,5-tetrazine (DPDHT). Synthesis and molecular structure of [(DPT)(GaMe2)2]
Preston, Peter N.,Rettig, Steven J.,Storr, Alan,Trotter, James
, p. 1800 - 1804 (1998)
The facile reaction of 3,6-di(2-pyridyl)-1,4-dihydro-1,2,4,5-tetrazine (DPDHT) (1) with trimethylgallium has resulted in the formation of the purple crystalline product, [(DPT)(GaMe2)2] (2), via methane elimination. Crystals of [(DPT)(GaMe2)2] are orthorhombic, Pbca, a = 15.380(2), b = 21.642(4), c = 11.355(2) A, Z = 8. The structure was solved by heavy-atom Patterson methods and refined by full-matrix least-squares procedures to R = 0.035 for 1570 reflections with I ≥ 3σ(I) (Rw = 0.063 for all 4342 reflections). The [(DPT)(GaMe2)2] molecule is roughly planar (apart from the four methyl groups), in contrast to the folded structure of the DPDHT molecule; molecular dimensions are normal.
Aryl-NHC-group 13 trimethyl complexes: structural, stability and bonding insights
Wu, Melissa M.,Gill, Arran M.,Yunpeng, Lu,Yongxin, Li,Ganguly, Rakesh,Falivene, Laura,García, Felipe
, p. 854 - 864 (2017)
Treatment of aromatic N-substituted N-heterocyclic carbenes (NHCs) with trimethyl-gallium and -indium yielded the new Lewis acid-base adducts, IMes·GaMe3 (1), SIMes·GaMe3 (2), IPr·GaMe3 (3), SIPr·GaMe3 (4), IMes·InMe3 (5), SIMes·InMe3 (6), IPr·InMe3 (7), and SIPr·InMe3 (8), with all complexes being identified by X-ray diffraction, IR, and multinuclear NMR analyses. Complex stability was found to be largely dependent on the nature of the constituent NHC ligands. Percent buried volume (%VBur) and topographic steric map analyses were employed to quantify and elucidate the observed trends. Additionally, a detailed bond snapping energy (BSE) decomposition analysis focusing on both steric and orbital interactions of the M-NHC bond (M = Al, Ga and In) has been performed.
Homoleptic and heteroleptic gallium(III) compounds containing monosubstituted cyclopentadienyl ligands: Ga(C5H4Me)3, Ga(C5H4SiMe3)3, and R2Ga(C5H4
Beachley Jr.,Mosscrop, Michael T.
, p. 4550 - 4556 (2000)
The new gallium(III) cyclopentadienyl derivatives Ga(C5H4Me)3 and Ga(C5SiMe3)3 have been synthesized by metathetical reactions. Subsequent stoichiometric ligand redistribution reactions wit
Reactivity of carbonyl-functionalized phosphaalkenes RC(O)P=C(NMe2)2 (R = tBu, ph) towards electrophiles
Weber, Lothar,Uthmann, Stefan,Stammler, Hans-Georg,Neumann, Beate,Schoeller, Wolfgang W.,Boese, Roland,Bl?ser, Dieter
, p. 2369 - 2381 (1999)
The reaction of the carbonyl-functionalized phosphaalkenes RC(O)P=C(NMe2)2 [R = tBu (2a), Ph (2b)] with protic acids and alkylating reagents occurred at the two-coordinate phosphorus atom to give the phosphanyl-substituted carbocations 3a,b and 4a,b. In contrast, treatment with Me3SiOSO2CF3 resulted in attack at the oxygen atom by the silyl group, and the formation of [RC(OSiMe3)= PC(NMe2)2]SO3CF3 (5a,b). Similarly, the Lewis acids B(C6F5)3, Al(tBu)2Cl and AlMe3 were ligated to the oxygen atom of the carbonyl group. Two equivalents of GaMe3 were added to the oxygen and phosphorus atom of the phosphaalkene to yield the thermolabile complexes [RC(OGaMe3)=P(GaMe3)C(NMe2)2] (10a,b). In contrast, one molecule of InMe3 was bound to the phosphorus center of the phosphorus compound. Reaction of the phosphaalkenes with [Ni(CO)4], [Fe2(CO)9] or [{(Z)-cyclooctene}Cr(CO)5] also took place at the pnictogen atom, resulting in complexes of the type [RC(O)P{M(CO)(n)}C(NMe2)2] (R = tBu, Ph; M = Ni, n = 3; Fe, n = 4; Cr, n = 5). The chemical transformations reported here underline the versatile chemistry of phosphaalkenes and emphasize a relationship between carbonyl- functionalized phosphaalkenes and the well-investigated class of phosphorus ylides. X-ray structures of compounds 6b, 7b*, 10a, 11a and 12a are reported.
A new synthetic route to trimethylgallium
Revin,Artemov,Sazonova
, p. 1359 - 1363 (2013)
A new synthetic route to trimethylgallium was developed. It is based on preparation of gallium methyl derivatives by the Green reaction, followed by their alkylation with methyl Grignard reagent. The suggested procedure is well reproducible, with the yield of pure trimethylgallium exceeding 90%.
Polymorphism in the crystal structures of the group 13 trimethyls
Boese, Roland,Downs, Anthony J.,Greene, Timothy M.,Hall, Alexander W.,Morrison, Carole A.,Parsons, Simon
, p. 2450 - 2457 (2003)
Crystal structure have been determined for trimethylboron, BMe3, and for a new polymorph of trimethylgallium, GaMe3; in addition, the crystal structure of trimethylthallium, TlMe3, has been redetermined. The BMe3 crystal structure represents a new structural type for the group 13 trimethyl derivatives in the solid state. In contrast to its heavier analogues, it consists of layer containing only very weakly interacting BMe3 molecules. GaMe3 forms a ladder-like pseudo-polymer via long gallium-to-methyl intermolecular interactions with Ga...C distances in the range 3.096(3)-3.226(4) A. This is compared with a recently reported crystal structure of a polymorph, which, like InMe3 and TlMe3, is characterized by the formation of pseudo-tetramers. The effects of crystallization and secondary interactions have been analyzed by comparison with related crystallographic, gas-phase electron diffraction, and spectroscopic studies of these and other trimethyl derivatives of the group 13 elements. The energetic differences between polymorphs of BMe3, GaMe3, and InMe3 have been explored by plane wave DFT calculations. The energy differences between the BMe3-like layered structure and the InMe3-like pseudo-tetrameric structure are calculated to be -1.7, +3.6, and +10.4 kJ mol-1 for BMe3, GaMe3, and InMe3, respectively.
71Ga NMR studies of mixtures of gallium trichloride and trimethylgallium
Cerny, Z.,Machacek, J.,Fusek, J.,Kriz, O.,Casensky, B.,Tuck, Dennis G.
, p. 25 - 30 (1993)
71Ga NMR spectra of solutions of GaCl3 and Me3Ga, and of binary mixtures of GaCl3-Me3Ga, in n-heptane have been recorded.The resonance signals for both Me3Ga and GaCl3 are unchanged on dilution over the temperature range 20-100 deg C.Mixtures of GaCl3 and Me3Ga show only one resonance signal, whose chemical shift is determined predominantly by the nature of the coordination at gallium, indicating rapid chemical exchange of the species involved.The results of studies of methanolysis and hydrolysis, and of adduct formation, are also discussed.The 71Ga resonances of several possible external standards in the temperature range 20-100 deg C are also reported.The 71Ga NMR signal of a solution of GaCl4- in 6 M aqueous hydrochloric acid, for which δ(71Ga) = 250 +/- 0.5 ppm downfield from the signal of a 1 M solution of 3+3- in 1 M HClO4, is recommended as a temperature-independent external standard for gallium NMR studies.
Process for preparing alkyl metal compounds
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Paragraph 0122-0125, (2020/05/30)
The invention relates to a method for producing alkyl metal compounds, starting materials for the production of trialkyl gallium and trialkyl indium comprise metallic indium or metallic gallium, at least one alkyl donor, a reducing agent and a solvent; the alkyl donor is alkyl halide; R in MR 2-4 represents alkyl group, 2 to 4 R groups are independently selected from the same or different alkyl groups; M is especially aluminum, gallium or indium; high purity gallium or indium or aluminum is used; sesquialkyl aluminum chloride is used as a reaction promoter, and the metal gallium or metal indium is reacted with alkyl chloride of the alkyl donor at low temperature and low pressure to generate sesquialkyl gallium chloride or sesquialkyl indium chloride; when the sesquialkyl gallium chloride or indium sesquialkyl chloride is reduced to the trialkyl gallium or trialkyl indium by a reducing agent, metal gallium or metal indium is necessarily generated simultaneously; the newly generated metal gallium or metal indium reacts with chloromethane (ethyl) in situ, so that the starting materials are fully utilized. The yield of the two steps is almost complete. The new synthetic route is an environment-friendly green process.
