A novel group of alkaline earth metal amides: Syntheses and characterization of M[N(2,6-iPr2C6H3) (SiMe3)]2(THF)2 (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-iPr2C6H3) (SiMe3)]2

Wilda Vargas; Ulrich Englich; Karin Ruhlandt-Senge

doi:10.1021/ic0203668

A novel group of alkaline earth metal amides: Syntheses and characterization of M[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂(THF)₂ (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂

Wilda Vargas, Ulrich Englich, Karin Ruhlandt-Senge

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

73 Scopus citations

Abstract

Novel alkaline earth metal aryl-substituted silylamides were prepared using alkane (Mg) and salt elimination reactions (Mg, Ca, Sr, and Ba). The salt elimination regime involved the treatment of the alkaline earth metal iodides with 2 equiv of the respective potassium amide KNDiip(SiMe₃), (Diip = 2,6-i-Pr₂C₆H₃). The organomagnesium source for the alkane elimination was (ⁿBu/^SBu)₂Mg. All compounds were characterized using ¹H, ¹³C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDilp(SiMe₃)]₂THF₂). Crystal data with Mo Kα (λ = 0.710 73 Å) are as follows: Mg[NDiip(SiMe₃)]₂, 1, a = 9.4687(6) Å, b = 9.6818(6) Å, c = 17.9296(1) Å, (α = 96.487(1)°, β = 94.537(1)°, γ = 89.222(1)°, V = 1608.8(2) Å³, Z = 2 (two independent molecules), triclinic, space group P1̄, R1 (all data) 0.0508; ⁿBuMg[NDiip(SiMe₃)]THF₂, 2, a = 9.5413(1) Å, b = 16.493(2) Å, c = 9.8218(1) Å, β = 108.149(2)°, V = 1468.7(4) Å³, Z = 2, monoclinic, space group P2₁, R1(all data) = 0.1232; Ca[NDiip(SiMe₃)]₂THF₂, 4, a = 9.7074(1) Å, b = 20.9466(4) Å, c = 21.6242(3) Å, α = 73.573(1)°, β = 78.632-(1)°, γ = 89.621(1)°, V = 4129.1(1) Å³, Z = 4 (two independent molecules), triclinic, space group P1̄, R1 (all data) = 0.0902; Sr[NDiip(SiMe₃)]₂THF₂, 5, a = 20.5874(5) Å, b = 9.8785(2) Å, c = 20.8522(5) Å, β = 102.035-(2)°, V = 4147.6(2) Å³, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe₃)]₂THF₂, 6, a = 20.5476(2) Å, b = 10.0353(2) Å, c = 20.9020(4) Å, β = 101.657(1)°, V = 4221.0(1) Å³, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.

Original language	English (US)
Pages (from-to)	5602-5608
Number of pages	7
Journal	Inorganic Chemistry
Volume	41
Issue number	21
DOIs	https://doi.org/10.1021/ic0203668
State	Published - Oct 21 2002

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Physical and Theoretical Chemistry
Inorganic Chemistry

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A novel group of alkaline earth metal amides: Syntheses and characterization of M[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂(THF)₂ (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂. / Vargas, Wilda; Englich, Ulrich ; Ruhlandt-Senge, Karin.
In: Inorganic Chemistry, Vol. 41, No. 21, 21.10.2002, p. 5602-5608.

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

@article{59d43b81dcf24e8b9a5ecf539cf8ee5e,

title = "A novel group of alkaline earth metal amides: Syntheses and characterization of M[N(2,6-iPr2C6H3) (SiMe3)]2(THF)2 (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-iPr2C6H3) (SiMe3)]2",

abstract = "Novel alkaline earth metal aryl-substituted silylamides were prepared using alkane (Mg) and salt elimination reactions (Mg, Ca, Sr, and Ba). The salt elimination regime involved the treatment of the alkaline earth metal iodides with 2 equiv of the respective potassium amide KNDiip(SiMe3), (Diip = 2,6-i-Pr2C6H3). The organomagnesium source for the alkane elimination was (nBu/SBu)2Mg. All compounds were characterized using 1H, 13C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDilp(SiMe3)]2THF2). Crystal data with Mo Kα (λ = 0.710 73 {\AA}) are as follows: Mg[NDiip(SiMe3)]2, 1, a = 9.4687(6) {\AA}, b = 9.6818(6) {\AA}, c = 17.9296(1) {\AA}, (α = 96.487(1)°, β = 94.537(1)°, γ = 89.222(1)°, V = 1608.8(2) {\AA}3, Z = 2 (two independent molecules), triclinic, space group P{\=1}, R1 (all data) 0.0508; nBuMg[NDiip(SiMe3)]THF2, 2, a = 9.5413(1) {\AA}, b = 16.493(2) {\AA}, c = 9.8218(1) {\AA}, β = 108.149(2)°, V = 1468.7(4) {\AA}3, Z = 2, monoclinic, space group P21, R1(all data) = 0.1232; Ca[NDiip(SiMe3)]2THF2, 4, a = 9.7074(1) {\AA}, b = 20.9466(4) {\AA}, c = 21.6242(3) {\AA}, α = 73.573(1)°, β = 78.632-(1)°, γ = 89.621(1)°, V = 4129.1(1) {\AA}3, Z = 4 (two independent molecules), triclinic, space group P{\=1}, R1 (all data) = 0.0902; Sr[NDiip(SiMe3)]2THF2, 5, a = 20.5874(5) {\AA}, b = 9.8785(2) {\AA}, c = 20.8522(5) {\AA}, β = 102.035-(2)°, V = 4147.6(2) {\AA}3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe3)]2THF2, 6, a = 20.5476(2) {\AA}, b = 10.0353(2) {\AA}, c = 20.9020(4) {\AA}, β = 101.657(1)°, V = 4221.0(1) {\AA}3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.",

author = "Wilda Vargas and Ulrich Englich and Karin Ruhlandt-Senge",

year = "2002",

month = oct,

day = "21",

doi = "10.1021/ic0203668",

language = "English (US)",

volume = "41",

pages = "5602--5608",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "21",

}

TY - JOUR

T1 - A novel group of alkaline earth metal amides

T2 - Syntheses and characterization of M[N(2,6-iPr2C6H3) (SiMe3)]2(THF)2 (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-iPr2C6H3) (SiMe3)]2

AU - Vargas, Wilda

AU - Englich, Ulrich

AU - Ruhlandt-Senge, Karin

PY - 2002/10/21

Y1 - 2002/10/21

N2 - Novel alkaline earth metal aryl-substituted silylamides were prepared using alkane (Mg) and salt elimination reactions (Mg, Ca, Sr, and Ba). The salt elimination regime involved the treatment of the alkaline earth metal iodides with 2 equiv of the respective potassium amide KNDiip(SiMe3), (Diip = 2,6-i-Pr2C6H3). The organomagnesium source for the alkane elimination was (nBu/SBu)2Mg. All compounds were characterized using 1H, 13C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDilp(SiMe3)]2THF2). Crystal data with Mo Kα (λ = 0.710 73 Å) are as follows: Mg[NDiip(SiMe3)]2, 1, a = 9.4687(6) Å, b = 9.6818(6) Å, c = 17.9296(1) Å, (α = 96.487(1)°, β = 94.537(1)°, γ = 89.222(1)°, V = 1608.8(2) Å3, Z = 2 (two independent molecules), triclinic, space group P1̄, R1 (all data) 0.0508; nBuMg[NDiip(SiMe3)]THF2, 2, a = 9.5413(1) Å, b = 16.493(2) Å, c = 9.8218(1) Å, β = 108.149(2)°, V = 1468.7(4) Å3, Z = 2, monoclinic, space group P21, R1(all data) = 0.1232; Ca[NDiip(SiMe3)]2THF2, 4, a = 9.7074(1) Å, b = 20.9466(4) Å, c = 21.6242(3) Å, α = 73.573(1)°, β = 78.632-(1)°, γ = 89.621(1)°, V = 4129.1(1) Å3, Z = 4 (two independent molecules), triclinic, space group P1̄, R1 (all data) = 0.0902; Sr[NDiip(SiMe3)]2THF2, 5, a = 20.5874(5) Å, b = 9.8785(2) Å, c = 20.8522(5) Å, β = 102.035-(2)°, V = 4147.6(2) Å3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe3)]2THF2, 6, a = 20.5476(2) Å, b = 10.0353(2) Å, c = 20.9020(4) Å, β = 101.657(1)°, V = 4221.0(1) Å3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.

AB - Novel alkaline earth metal aryl-substituted silylamides were prepared using alkane (Mg) and salt elimination reactions (Mg, Ca, Sr, and Ba). The salt elimination regime involved the treatment of the alkaline earth metal iodides with 2 equiv of the respective potassium amide KNDiip(SiMe3), (Diip = 2,6-i-Pr2C6H3). The organomagnesium source for the alkane elimination was (nBu/SBu)2Mg. All compounds were characterized using 1H, 13C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDilp(SiMe3)]2THF2). Crystal data with Mo Kα (λ = 0.710 73 Å) are as follows: Mg[NDiip(SiMe3)]2, 1, a = 9.4687(6) Å, b = 9.6818(6) Å, c = 17.9296(1) Å, (α = 96.487(1)°, β = 94.537(1)°, γ = 89.222(1)°, V = 1608.8(2) Å3, Z = 2 (two independent molecules), triclinic, space group P1̄, R1 (all data) 0.0508; nBuMg[NDiip(SiMe3)]THF2, 2, a = 9.5413(1) Å, b = 16.493(2) Å, c = 9.8218(1) Å, β = 108.149(2)°, V = 1468.7(4) Å3, Z = 2, monoclinic, space group P21, R1(all data) = 0.1232; Ca[NDiip(SiMe3)]2THF2, 4, a = 9.7074(1) Å, b = 20.9466(4) Å, c = 21.6242(3) Å, α = 73.573(1)°, β = 78.632-(1)°, γ = 89.621(1)°, V = 4129.1(1) Å3, Z = 4 (two independent molecules), triclinic, space group P1̄, R1 (all data) = 0.0902; Sr[NDiip(SiMe3)]2THF2, 5, a = 20.5874(5) Å, b = 9.8785(2) Å, c = 20.8522(5) Å, β = 102.035-(2)°, V = 4147.6(2) Å3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe3)]2THF2, 6, a = 20.5476(2) Å, b = 10.0353(2) Å, c = 20.9020(4) Å, β = 101.657(1)°, V = 4221.0(1) Å3, Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.

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JO - Inorganic Chemistry

JF - Inorganic Chemistry

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A novel group of alkaline earth metal amides: Syntheses and characterization of M[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂(THF)₂ (M = Mg, Ca, Sr, Ba) and the linear, two-coordinate Mg[N(2,6-ⁱPr₂C₆H₃) (SiMe₃)]₂

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