Lewis base adduct stabilized organogallium azides: Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas

Alexander Miehr; Mike R. Mattner; Roland A. Fischer

doi:10.1021/om950926t

Lewis base adduct stabilized organogallium azides: Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas

Alexander Miehr
, Mike R. Mattner
, Roland A. Fischer

Chair of Inorganic and Organometallic Chemistry

Technical University of Munich
Heidelberg University

Research output: Contribution to journal › Article › peer-review

54 Scopus citations

Abstract

The organogallium azides (N₃)_2-a(R)_aGa[(CH₂) ₃NMe₂]_1-a (1a-c: R = CH₃, ^tBu; a = 0, 1), (Et)(N₃)₂Ga (2a), and (Et)(N₃)₂Ga·L (2b-d: L = thf, H₂N^tBu, py, NC₇H₁₃) are quantitatively synthesized by salt metathesis from the chloro species (Cl)_2-a(R)_aGa[(CH₂)₃NMe ₂]_1-a (a = 0, 1) or EtGaCl₂ and sodium azide. The preferential ammonolysis of Ga-N₃ bonds for [Et₂Ga(N₃)]₃ (4) and 1 and 2 is demonstrated; e.g. the dimer Et₂Ga(μ-NH₂)(μ-N₃)GaEt₂ (3) was obtained. The characterization of these compounds by means of elemental analysis, ¹H-, ¹³C-, ¹⁴N-, and ¹⁵N-NMR, MS, and infrared v(N₃) data is reported. The dynamics of the intramolecular Ga-N donor-acceptor bonded heterocycle and the azide group is discussed on the basis of variable-temperature NMR data. The barrier of activation of the bimolecular azide exchange process for (N₃)₂Ga[(CH₂)₃NMe₂] (1c) amounts about 50 kJ·mol^-1. The role of ammonia as reactive carrier gas for low-pressure metal organic chemical vapor deposition (MOCVD) of GaN with 1c as precursor is discussed.

Original language	English
Pages (from-to)	2053-2059
Number of pages	7
Journal	Organometallics
Volume	15
Issue number	8
DOIs	https://doi.org/10.1021/om950926t
State	Published - 16 Apr 1996

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@article{e9d00152f5e5435f8e783aba655f4150,

title = "Lewis base adduct stabilized organogallium azides: Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas",

abstract = "The organogallium azides (N3)2-a(R)aGa[(CH2) 3NMe2]1-a (1a-c: R = CH3, tBu; a = 0, 1), (Et)(N3)2Ga (2a), and (Et)(N3)2Ga·L (2b-d: L = thf, H2NtBu, py, NC7H13) are quantitatively synthesized by salt metathesis from the chloro species (Cl)2-a(R)aGa[(CH2)3NMe 2]1-a (a = 0, 1) or EtGaCl2 and sodium azide. The preferential ammonolysis of Ga-N3 bonds for [Et2Ga(N3)]3 (4) and 1 and 2 is demonstrated; e.g. the dimer Et2Ga(μ-NH2)(μ-N3)GaEt2 (3) was obtained. The characterization of these compounds by means of elemental analysis, 1H-, 13C-, 14N-, and 15N-NMR, MS, and infrared v(N3) data is reported. The dynamics of the intramolecular Ga-N donor-acceptor bonded heterocycle and the azide group is discussed on the basis of variable-temperature NMR data. The barrier of activation of the bimolecular azide exchange process for (N3)2Ga[(CH2)3NMe2] (1c) amounts about 50 kJ·mol-1. The role of ammonia as reactive carrier gas for low-pressure metal organic chemical vapor deposition (MOCVD) of GaN with 1c as precursor is discussed.",

author = "Alexander Miehr and Mattner, \{Mike R.\} and Fischer, \{Roland A.\}",

year = "1996",

month = apr,

day = "16",

doi = "10.1021/om950926t",

language = "English",

volume = "15",

pages = "2053--2059",

journal = "Organometallics",

issn = "0276-7333",

publisher = "American Chemical Society",

number = "8",

}

Lewis base adduct stabilized organogallium azides: Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas. / Miehr, Alexander; Mattner, Mike R.; Fischer, Roland A.
In: Organometallics, Vol. 15, No. 8, 16.04.1996, p. 2053-2059.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Lewis base adduct stabilized organogallium azides

T2 - Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas

AU - Miehr, Alexander

AU - Mattner, Mike R.

AU - Fischer, Roland A.

PY - 1996/4/16

Y1 - 1996/4/16

N2 - The organogallium azides (N3)2-a(R)aGa[(CH2) 3NMe2]1-a (1a-c: R = CH3, tBu; a = 0, 1), (Et)(N3)2Ga (2a), and (Et)(N3)2Ga·L (2b-d: L = thf, H2NtBu, py, NC7H13) are quantitatively synthesized by salt metathesis from the chloro species (Cl)2-a(R)aGa[(CH2)3NMe 2]1-a (a = 0, 1) or EtGaCl2 and sodium azide. The preferential ammonolysis of Ga-N3 bonds for [Et2Ga(N3)]3 (4) and 1 and 2 is demonstrated; e.g. the dimer Et2Ga(μ-NH2)(μ-N3)GaEt2 (3) was obtained. The characterization of these compounds by means of elemental analysis, 1H-, 13C-, 14N-, and 15N-NMR, MS, and infrared v(N3) data is reported. The dynamics of the intramolecular Ga-N donor-acceptor bonded heterocycle and the azide group is discussed on the basis of variable-temperature NMR data. The barrier of activation of the bimolecular azide exchange process for (N3)2Ga[(CH2)3NMe2] (1c) amounts about 50 kJ·mol-1. The role of ammonia as reactive carrier gas for low-pressure metal organic chemical vapor deposition (MOCVD) of GaN with 1c as precursor is discussed.

AB - The organogallium azides (N3)2-a(R)aGa[(CH2) 3NMe2]1-a (1a-c: R = CH3, tBu; a = 0, 1), (Et)(N3)2Ga (2a), and (Et)(N3)2Ga·L (2b-d: L = thf, H2NtBu, py, NC7H13) are quantitatively synthesized by salt metathesis from the chloro species (Cl)2-a(R)aGa[(CH2)3NMe 2]1-a (a = 0, 1) or EtGaCl2 and sodium azide. The preferential ammonolysis of Ga-N3 bonds for [Et2Ga(N3)]3 (4) and 1 and 2 is demonstrated; e.g. the dimer Et2Ga(μ-NH2)(μ-N3)GaEt2 (3) was obtained. The characterization of these compounds by means of elemental analysis, 1H-, 13C-, 14N-, and 15N-NMR, MS, and infrared v(N3) data is reported. The dynamics of the intramolecular Ga-N donor-acceptor bonded heterocycle and the azide group is discussed on the basis of variable-temperature NMR data. The barrier of activation of the bimolecular azide exchange process for (N3)2Ga[(CH2)3NMe2] (1c) amounts about 50 kJ·mol-1. The role of ammonia as reactive carrier gas for low-pressure metal organic chemical vapor deposition (MOCVD) of GaN with 1c as precursor is discussed.

UR - https://www.scopus.com/pages/publications/0000164534

U2 - 10.1021/om950926t

DO - 10.1021/om950926t

M3 - Article

AN - SCOPUS:0000164534

SN - 0276-7333

VL - 15

SP - 2053

EP - 2059

JO - Organometallics

JF - Organometallics

IS - 8

ER -

Lewis base adduct stabilized organogallium azides: Synthesis and dynamic NMR spectroscopic studies of novel precursors to gallium nitride and role of ammonia as reactive carrier gas

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