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Title: Synthesis and structural characterization of the beryllium compounds [Be(2,4,6-Me[sub 3]C[sub 6]H[sub 2])[sub 2](OEt[sub 2])], [Be[l brace]O(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](OEt[sub 2])], and [Be[l brace]S(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](THF)][center dot]PhMe and determination of the structure of [BeCl[sub 2](OEt[sub 2])[sub 2]]

Abstract

The preparations of some new classes of beryllium compounds that have a coordination number of 3 at beryllium are reported. They were synthesized by the reaction of BeCl[sub 2](OEt[sub 2])[sub 2] with the appropriate lithium salt to give the products [BeMes[sub 2](OEt[sub 2])] (1; Mes = 2,4,6-Me[sub 3]C[sub 6]H[sub 2]), [Be(OMes*)[sub 2](OEt[sub 2])] (2; Mes* = 2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2]), and [Be(SMes*)[sub 2](THF)][center dot]PhMe (3). The compounds were characterized by [sup 1]H NMR and IR spectroscopy, C and H analysis, and X-ray crystallography. The crystal structure of [BeCl[sub 2](OEt[sub 2])[sub 2]] (4) was also determined. Crystal data (Mo K[alpha] ([lambda] = 0.710 69 [Angstrom]) at 130 K) are as follows: [BeMes[sub 2](OEt[sub 2])] (1), a = 11.913(3) [Angstrom], c = 28.390(8) [Angstrom], V = 4029(2) [Angstrom][sup 3], tetragonal, space group I[bar 4]2m, 975 (I > 3[sigma](I)) data, R = 0.042; [Be(OMes*)[sub 2]OEt[sub 2]] (2), a = 25.022(9) [Angstrom], b = 9.834(3) [Angstrom], c = 16.290(4) [Angstrom], [beta] = 96.48(3)[degrees], V = 3982(2) [Angstrom][sup 3], monoclinic, space group C2/c, 3173 (I > 3[sigma](I)) data, R = 0.051; [Be(SMes*)[sub 2]THF][center dot]PhMe (3), a = 8.695(4) [Angstrom], b = 17.399(10) [Angstrom], c = 17.437(8) [Angstrom], [alpha] = 60.80(4)[degrees], [beta] = 83.29(4)[degrees], [gamma] =more » 84.24(4)[degrees], V = 2284(2) [Angstrom][sup 3], triclinic, space group P[bar 1], 3751 (I > 2[sigma](I)) data, R = 0.061; [BeCl[sub 2](OEt[sub 2])[sub 2]] (4), a = 7.486(3) [Angstrom], c = 20.022(8) [Angstrom], V = 971.7(6) [Angstrom][sup 3], trigonal, space group P3[sub 1]2[sub 1], 646 (I > 2[sigma](I)) data, R = 0.028. 32 refs., 4 figs., 3 tabs.« less

Authors:
; ; ;  [1]
  1. Univ. of California, Davis (United States)
Publication Date:
OSTI Identifier:
6236468
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry; (United States)
Additional Journal Information:
Journal Volume: 32:9; Journal ID: ISSN 0020-1669
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; BERYLLIUM COMPLEXES; MOLECULAR STRUCTURE; ORGANOMETALLIC COMPOUNDS; ABSORPTION SPECTROSCOPY; ALKOXIDES; CHEMICAL PREPARATION; COORDINATION NUMBER; CRYSTAL STRUCTURE; LATTICE PARAMETERS; MONOCLINIC LATTICES; NUCLEAR MAGNETIC RESONANCE; TETRAGONAL LATTICES; TRICLINIC LATTICES; TRIGONAL LATTICES; X-RAY DIFFRACTION; ALKALINE EARTH METAL COMPLEXES; COHERENT SCATTERING; COMPLEXES; CRYSTAL LATTICES; DIFFRACTION; MAGNETIC RESONANCE; ORGANIC COMPOUNDS; RESONANCE; SCATTERING; SPECTROSCOPY; SYNTHESIS; 400201* - Chemical & Physicochemical Properties

Citation Formats

Ruhlandt-Senge, K, Bartlett, R A, Olmstead, M M, and Power, P P. Synthesis and structural characterization of the beryllium compounds [Be(2,4,6-Me[sub 3]C[sub 6]H[sub 2])[sub 2](OEt[sub 2])], [Be[l brace]O(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](OEt[sub 2])], and [Be[l brace]S(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](THF)][center dot]PhMe and determination of the structure of [BeCl[sub 2](OEt[sub 2])[sub 2]]. United States: N. p., 1993. Web. doi:10.1021/ic00061a031.
Ruhlandt-Senge, K, Bartlett, R A, Olmstead, M M, & Power, P P. Synthesis and structural characterization of the beryllium compounds [Be(2,4,6-Me[sub 3]C[sub 6]H[sub 2])[sub 2](OEt[sub 2])], [Be[l brace]O(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](OEt[sub 2])], and [Be[l brace]S(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](THF)][center dot]PhMe and determination of the structure of [BeCl[sub 2](OEt[sub 2])[sub 2]]. United States. https://doi.org/10.1021/ic00061a031
Ruhlandt-Senge, K, Bartlett, R A, Olmstead, M M, and Power, P P. 1993. "Synthesis and structural characterization of the beryllium compounds [Be(2,4,6-Me[sub 3]C[sub 6]H[sub 2])[sub 2](OEt[sub 2])], [Be[l brace]O(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](OEt[sub 2])], and [Be[l brace]S(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](THF)][center dot]PhMe and determination of the structure of [BeCl[sub 2](OEt[sub 2])[sub 2]]". United States. https://doi.org/10.1021/ic00061a031.
@article{osti_6236468,
title = {Synthesis and structural characterization of the beryllium compounds [Be(2,4,6-Me[sub 3]C[sub 6]H[sub 2])[sub 2](OEt[sub 2])], [Be[l brace]O(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](OEt[sub 2])], and [Be[l brace]S(2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2])[r brace][sub 2](THF)][center dot]PhMe and determination of the structure of [BeCl[sub 2](OEt[sub 2])[sub 2]]},
author = {Ruhlandt-Senge, K and Bartlett, R A and Olmstead, M M and Power, P P},
abstractNote = {The preparations of some new classes of beryllium compounds that have a coordination number of 3 at beryllium are reported. They were synthesized by the reaction of BeCl[sub 2](OEt[sub 2])[sub 2] with the appropriate lithium salt to give the products [BeMes[sub 2](OEt[sub 2])] (1; Mes = 2,4,6-Me[sub 3]C[sub 6]H[sub 2]), [Be(OMes*)[sub 2](OEt[sub 2])] (2; Mes* = 2,4,6-t-Bu[sub 3]C[sub 6]H[sub 2]), and [Be(SMes*)[sub 2](THF)][center dot]PhMe (3). The compounds were characterized by [sup 1]H NMR and IR spectroscopy, C and H analysis, and X-ray crystallography. The crystal structure of [BeCl[sub 2](OEt[sub 2])[sub 2]] (4) was also determined. Crystal data (Mo K[alpha] ([lambda] = 0.710 69 [Angstrom]) at 130 K) are as follows: [BeMes[sub 2](OEt[sub 2])] (1), a = 11.913(3) [Angstrom], c = 28.390(8) [Angstrom], V = 4029(2) [Angstrom][sup 3], tetragonal, space group I[bar 4]2m, 975 (I > 3[sigma](I)) data, R = 0.042; [Be(OMes*)[sub 2]OEt[sub 2]] (2), a = 25.022(9) [Angstrom], b = 9.834(3) [Angstrom], c = 16.290(4) [Angstrom], [beta] = 96.48(3)[degrees], V = 3982(2) [Angstrom][sup 3], monoclinic, space group C2/c, 3173 (I > 3[sigma](I)) data, R = 0.051; [Be(SMes*)[sub 2]THF][center dot]PhMe (3), a = 8.695(4) [Angstrom], b = 17.399(10) [Angstrom], c = 17.437(8) [Angstrom], [alpha] = 60.80(4)[degrees], [beta] = 83.29(4)[degrees], [gamma] = 84.24(4)[degrees], V = 2284(2) [Angstrom][sup 3], triclinic, space group P[bar 1], 3751 (I > 2[sigma](I)) data, R = 0.061; [BeCl[sub 2](OEt[sub 2])[sub 2]] (4), a = 7.486(3) [Angstrom], c = 20.022(8) [Angstrom], V = 971.7(6) [Angstrom][sup 3], trigonal, space group P3[sub 1]2[sub 1], 646 (I > 2[sigma](I)) data, R = 0.028. 32 refs., 4 figs., 3 tabs.},
doi = {10.1021/ic00061a031},
url = {https://www.osti.gov/biblio/6236468}, journal = {Inorganic Chemistry; (United States)},
issn = {0020-1669},
number = ,
volume = 32:9,
place = {United States},
year = {Wed Apr 28 00:00:00 EDT 1993},
month = {Wed Apr 28 00:00:00 EDT 1993}
}