Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu2(mpsa)2], [Cu6X2(mpsa)4] (X = Cl or Br), [Ag4(mpsa)4] and [(ZnEt)2(mpsa)2] [mpsa = 2-N(SiMe3)C5H3N-6-Me]

Lutz M. Engelhardt; Geraldine E. Jacobsen; Wyona C. Patalinghug; Brian W. Skelton; Colin L. Raston; Allan H. White

doi:10.1039/DT9910002859

Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]

Lutz M. Engelhardt, Geraldine E. Jacobsen, Wyona C. Patalinghug, Brian W. Skelton, Colin L. Raston, Allan H. White

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

30 Citations (Scopus)

Abstract

The copper(I) amide [Cu₂(mpsa)₂] 1 and its 1:1 adduct with CuX, [Cu₆(mpsa)₄X₂] (X = Cl, 2a or Br, 2b) {mpsa = [2-(6-methyl)pyridyl]trimethylsilylamido, 2-N(SiMe₃)C₅H₃N-6-Me}, the silver(I) amide [Ag₄(mpsa)₄] 3 and the zinc(II) amides [(ZnEt)₂(mpsa)₂] 4, [ZnCl(mpsa)] 5, and [Zn(mpsa)₂] 6, have been prepared from lithium reagents and the appropriate metal halide, and Hmpsa and ZnEt₂ (4 and 6). The amides 1-4 have been characterized crystallographically. In 1 the ligands span the two metal centres with Cu-N_amido 1.875(4), 1.887(4), Å, Cu-N_pyridyl 1.902(4), 1.903(4) Å, N-Cu-N 174.6(2), 173.4(2)°, and Cu ⋯ Cu 2.420(1) Å. Complexes 2a and 2b are isomorphous diethyl etherates; mpsa ligands span three metal centres with each N_amido bridging (i) a two-co-ordinate copper, the other co-ordination site being another N_amido, Cu-N 1.893(6)-1.927(7) Å, 2a, 1.884(9)-1.919(8) Å, 2b, and (ii) a three-co-ordinate copper bound by the amido centre, Cu-N, 2.100(6)-2.133(6) Å, 2a, 2.100(8)-2.152(9) Å, 2b, a pyridyl N-centre, 1.993(7)-2.006(7) Å, 2a, 1.983(9)-2.013(8) Å, 2b, and a halide, Cu-X 2.270(3)-2.303(3) Å, 2a, 2.409(3)-2.410(2) Å, 2b. Complex 3 is a hexane solvate; mpsa ligands link four silver atoms in plane; two silver atoms lie on a C₂ axis and are two-co-ordinate, bound by pairs of N_pyridyl groups; Ag-N, 2.140(3), 2.169(6) Å with N-Ag-N, 169.3(2), 171.2(2)°; the other (symmetry-related) pair are two-co-ordinate, bound by pairs of N_amido groups: Ag-N, 2.099(3), 2.097(4), with N-Ag-N, 168.6(2)°. In complex 4 the N_amido groups bridge the metal centres with N_pyridyl forming chelate rings on the same side of a Zn₂N₂ plane; Zn-N_pyridyl 2.125(5), 2.108(5) Å, Zn-N_amido 2.061(5), 2.072(5) Å (chelate ring), 2.245(5), 2.225(5) Å, Zn ⋯ Zn 2.958(2) Å. Compound 1 forms an adduct with trimethylphosphine, [Cu(mpsa)(PMe₃)₂] 7.

Original language	English
Pages (from-to)	2859-2868
Number of pages	10
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	11
DOIs	https://doi.org/10.1039/DT9910002859
Publication status	Published - Nov 1991
Externally published	Yes

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Engelhardt, L. M., Jacobsen, G. E., Patalinghug, W. C., Skelton, B. W., Raston, C. L., & White, A. H. (1991). Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]. Journal of the Chemical Society, Dalton Transactions, (11), 2859-2868. https://doi.org/10.1039/DT9910002859

Engelhardt, Lutz M. ; Jacobsen, Geraldine E. ; Patalinghug, Wyona C. ; Skelton, Brian W. ; Raston, Colin L. ; White, Allan H. / Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]. In: Journal of the Chemical Society, Dalton Transactions. 1991 ; No. 11. pp. 2859-2868.

@article{9892f5d033e74752bf01d3b53b8c5033,

title = "Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu2(mpsa)2], [Cu6X2(mpsa)4] (X = Cl or Br), [Ag4(mpsa)4] and [(ZnEt)2(mpsa)2] [mpsa = 2-N(SiMe3)C5H3N-6-Me]",

abstract = "The copper(I) amide [Cu2(mpsa)2] 1 and its 1:1 adduct with CuX, [Cu6(mpsa)4X2] (X = Cl, 2a or Br, 2b) {mpsa = [2-(6-methyl)pyridyl]trimethylsilylamido, 2-N(SiMe3)C5H3N-6-Me}, the silver(I) amide [Ag4(mpsa)4] 3 and the zinc(II) amides [(ZnEt)2(mpsa)2] 4, [ZnCl(mpsa)] 5, and [Zn(mpsa)2] 6, have been prepared from lithium reagents and the appropriate metal halide, and Hmpsa and ZnEt2 (4 and 6). The amides 1-4 have been characterized crystallographically. In 1 the ligands span the two metal centres with Cu-Namido 1.875(4), 1.887(4), {\AA}, Cu-Npyridyl 1.902(4), 1.903(4) {\AA}, N-Cu-N 174.6(2), 173.4(2)°, and Cu ⋯ Cu 2.420(1) {\AA}. Complexes 2a and 2b are isomorphous diethyl etherates; mpsa ligands span three metal centres with each Namido bridging (i) a two-co-ordinate copper, the other co-ordination site being another Namido, Cu-N 1.893(6)-1.927(7) {\AA}, 2a, 1.884(9)-1.919(8) {\AA}, 2b, and (ii) a three-co-ordinate copper bound by the amido centre, Cu-N, 2.100(6)-2.133(6) {\AA}, 2a, 2.100(8)-2.152(9) {\AA}, 2b, a pyridyl N-centre, 1.993(7)-2.006(7) {\AA}, 2a, 1.983(9)-2.013(8) {\AA}, 2b, and a halide, Cu-X 2.270(3)-2.303(3) {\AA}, 2a, 2.409(3)-2.410(2) {\AA}, 2b. Complex 3 is a hexane solvate; mpsa ligands link four silver atoms in plane; two silver atoms lie on a C2 axis and are two-co-ordinate, bound by pairs of Npyridyl groups; Ag-N, 2.140(3), 2.169(6) {\AA} with N-Ag-N, 169.3(2), 171.2(2)°; the other (symmetry-related) pair are two-co-ordinate, bound by pairs of Namido groups: Ag-N, 2.099(3), 2.097(4), with N-Ag-N, 168.6(2)°. In complex 4 the Namido groups bridge the metal centres with Npyridyl forming chelate rings on the same side of a Zn2N2 plane; Zn-Npyridyl 2.125(5), 2.108(5) {\AA}, Zn-Namido 2.061(5), 2.072(5) {\AA} (chelate ring), 2.245(5), 2.225(5) {\AA}, Zn ⋯ Zn 2.958(2) {\AA}. Compound 1 forms an adduct with trimethylphosphine, [Cu(mpsa)(PMe3)2] 7.",

author = "Engelhardt, {Lutz M.} and Jacobsen, {Geraldine E.} and Patalinghug, {Wyona C.} and Skelton, {Brian W.} and Raston, {Colin L.} and White, {Allan H.}",

year = "1991",

month = nov,

doi = "10.1039/DT9910002859",

language = "English",

pages = "2859--2868",

journal = "Journal of the Chemical Society, Dalton Transactions",

issn = "1470-479X",

number = "11",

}

Engelhardt, LM, Jacobsen, GE, Patalinghug, WC, Skelton, BW, Raston, CL & White, AH 1991, 'Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]', Journal of the Chemical Society, Dalton Transactions, no. 11, pp. 2859-2868. https://doi.org/10.1039/DT9910002859

Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]. / Engelhardt, Lutz M.; Jacobsen, Geraldine E.; Patalinghug, Wyona C.; Skelton, Brian W.; Raston, Colin L.; White, Allan H.

In: Journal of the Chemical Society, Dalton Transactions, No. 11, 11.1991, p. 2859-2868.

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

TY - JOUR

T1 - Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu2(mpsa)2], [Cu6X2(mpsa)4] (X = Cl or Br), [Ag4(mpsa)4] and [(ZnEt)2(mpsa)2] [mpsa = 2-N(SiMe3)C5H3N-6-Me]

AU - Engelhardt, Lutz M.

AU - Jacobsen, Geraldine E.

AU - Patalinghug, Wyona C.

AU - Skelton, Brian W.

AU - Raston, Colin L.

AU - White, Allan H.

PY - 1991/11

Y1 - 1991/11

N2 - The copper(I) amide [Cu2(mpsa)2] 1 and its 1:1 adduct with CuX, [Cu6(mpsa)4X2] (X = Cl, 2a or Br, 2b) {mpsa = [2-(6-methyl)pyridyl]trimethylsilylamido, 2-N(SiMe3)C5H3N-6-Me}, the silver(I) amide [Ag4(mpsa)4] 3 and the zinc(II) amides [(ZnEt)2(mpsa)2] 4, [ZnCl(mpsa)] 5, and [Zn(mpsa)2] 6, have been prepared from lithium reagents and the appropriate metal halide, and Hmpsa and ZnEt2 (4 and 6). The amides 1-4 have been characterized crystallographically. In 1 the ligands span the two metal centres with Cu-Namido 1.875(4), 1.887(4), Å, Cu-Npyridyl 1.902(4), 1.903(4) Å, N-Cu-N 174.6(2), 173.4(2)°, and Cu ⋯ Cu 2.420(1) Å. Complexes 2a and 2b are isomorphous diethyl etherates; mpsa ligands span three metal centres with each Namido bridging (i) a two-co-ordinate copper, the other co-ordination site being another Namido, Cu-N 1.893(6)-1.927(7) Å, 2a, 1.884(9)-1.919(8) Å, 2b, and (ii) a three-co-ordinate copper bound by the amido centre, Cu-N, 2.100(6)-2.133(6) Å, 2a, 2.100(8)-2.152(9) Å, 2b, a pyridyl N-centre, 1.993(7)-2.006(7) Å, 2a, 1.983(9)-2.013(8) Å, 2b, and a halide, Cu-X 2.270(3)-2.303(3) Å, 2a, 2.409(3)-2.410(2) Å, 2b. Complex 3 is a hexane solvate; mpsa ligands link four silver atoms in plane; two silver atoms lie on a C2 axis and are two-co-ordinate, bound by pairs of Npyridyl groups; Ag-N, 2.140(3), 2.169(6) Å with N-Ag-N, 169.3(2), 171.2(2)°; the other (symmetry-related) pair are two-co-ordinate, bound by pairs of Namido groups: Ag-N, 2.099(3), 2.097(4), with N-Ag-N, 168.6(2)°. In complex 4 the Namido groups bridge the metal centres with Npyridyl forming chelate rings on the same side of a Zn2N2 plane; Zn-Npyridyl 2.125(5), 2.108(5) Å, Zn-Namido 2.061(5), 2.072(5) Å (chelate ring), 2.245(5), 2.225(5) Å, Zn ⋯ Zn 2.958(2) Å. Compound 1 forms an adduct with trimethylphosphine, [Cu(mpsa)(PMe3)2] 7.

AB - The copper(I) amide [Cu2(mpsa)2] 1 and its 1:1 adduct with CuX, [Cu6(mpsa)4X2] (X = Cl, 2a or Br, 2b) {mpsa = [2-(6-methyl)pyridyl]trimethylsilylamido, 2-N(SiMe3)C5H3N-6-Me}, the silver(I) amide [Ag4(mpsa)4] 3 and the zinc(II) amides [(ZnEt)2(mpsa)2] 4, [ZnCl(mpsa)] 5, and [Zn(mpsa)2] 6, have been prepared from lithium reagents and the appropriate metal halide, and Hmpsa and ZnEt2 (4 and 6). The amides 1-4 have been characterized crystallographically. In 1 the ligands span the two metal centres with Cu-Namido 1.875(4), 1.887(4), Å, Cu-Npyridyl 1.902(4), 1.903(4) Å, N-Cu-N 174.6(2), 173.4(2)°, and Cu ⋯ Cu 2.420(1) Å. Complexes 2a and 2b are isomorphous diethyl etherates; mpsa ligands span three metal centres with each Namido bridging (i) a two-co-ordinate copper, the other co-ordination site being another Namido, Cu-N 1.893(6)-1.927(7) Å, 2a, 1.884(9)-1.919(8) Å, 2b, and (ii) a three-co-ordinate copper bound by the amido centre, Cu-N, 2.100(6)-2.133(6) Å, 2a, 2.100(8)-2.152(9) Å, 2b, a pyridyl N-centre, 1.993(7)-2.006(7) Å, 2a, 1.983(9)-2.013(8) Å, 2b, and a halide, Cu-X 2.270(3)-2.303(3) Å, 2a, 2.409(3)-2.410(2) Å, 2b. Complex 3 is a hexane solvate; mpsa ligands link four silver atoms in plane; two silver atoms lie on a C2 axis and are two-co-ordinate, bound by pairs of Npyridyl groups; Ag-N, 2.140(3), 2.169(6) Å with N-Ag-N, 169.3(2), 171.2(2)°; the other (symmetry-related) pair are two-co-ordinate, bound by pairs of Namido groups: Ag-N, 2.099(3), 2.097(4), with N-Ag-N, 168.6(2)°. In complex 4 the Namido groups bridge the metal centres with Npyridyl forming chelate rings on the same side of a Zn2N2 plane; Zn-Npyridyl 2.125(5), 2.108(5) Å, Zn-Namido 2.061(5), 2.072(5) Å (chelate ring), 2.245(5), 2.225(5) Å, Zn ⋯ Zn 2.958(2) Å. Compound 1 forms an adduct with trimethylphosphine, [Cu(mpsa)(PMe3)2] 7.

UR - http://www.scopus.com/inward/record.url?scp=37049068949&partnerID=8YFLogxK

U2 - 10.1039/DT9910002859

DO - 10.1039/DT9910002859

M3 - Article

AN - SCOPUS:37049068949

SP - 2859

EP - 2868

JO - Journal of the Chemical Society, Dalton Transactions

JF - Journal of the Chemical Society, Dalton Transactions

SN - 1470-479X

IS - 11

ER -

Engelhardt LM, Jacobsen GE, Patalinghug WC, Skelton BW, Raston CL, White AH. Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]. Journal of the Chemical Society, Dalton Transactions. 1991 Nov;(11):2859-2868. https://doi.org/10.1039/DT9910002859

Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu2(mpsa)2], [Cu6X2(mpsa)4] (X = Cl or Br), [Ag4(mpsa)4] and [(ZnEt)2(mpsa)2] [mpsa = 2-N(SiMe3)C5H3N-6-Me]

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Synthesis and structure of copper(I), silver(I) and zinc(II) amides [cu₂(mpsa)₂], [Cu₆X₂(mpsa)₄] (X = Cl or Br), [Ag₄(mpsa)₄] and [(ZnEt)₂(mpsa)₂] [mpsa = 2-N(SiMe₃)C₅H₃N-6-Me]