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
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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一组新型碱土金属酰胺：M[N(2,6-iPr2C6H3)(SiMe3)]2(THF)2 (M = Mg, Ca, Sr, Ba) 和线性二配位化合物的合成和表征
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发表时间：
2002
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通讯作者：
K. Ruhlandt
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作者：
Wilda Vargas;U. Englich;K. Ruhlandt
采用烷烃（Mg）和盐消除反应（Mg、Ca、Sr和Ba）制备了新型碱土金属芳基取代的甲硅烷基酰胺。除盐方案涉及用2当量的相应氨基化钾KNDiip（SiMe（3））（Diip = 2，6-i-Pr（2）C（6）H（3））处理碱土金属碘化物。消除烷烃的有机镁源为（（n）（）Bu/（s）（）Bu）（2）Mg。除了X射线晶体学（Mg[NDiip（SiMe（3））]（2）THF（2）除外）之外，所有化合物均使用（1）H、（13）C NMR和IR光谱进行表征。晶体数据与Mo Kalalpha（λ = 0.710 73 A）的值如下：Mg[NDiip（SiMe（3））]（2），1，a = 9.4687（6）A，B = 9.6818（6）A，c = 17.9296（1）A，α = 96.487（1）度，β = 94.537（1）度，γ = 89.222（1）度，V = 1608.8（2）A（3），Z = 2（两个独立分子），三斜晶系，空间群P（-）1，R1（所有数据）= 0.0508;（n）（）BuMg[NDiip（SiMe（3））]THF（2），2，a = 9.5413（1）A，B = 16.493（2）A，c = 9.8218（1）A，β = 108.149（2）度，V = 1468.7（4）A（3），Z = 2，单斜晶系，空间群P2（1），R1（所有数据）= 0.1232; Ca[NDiip（SiMe（3））]（2）THF（2），4，a = 9.7074（1）A，B = 20.9466（4）A，c = 21.6242（3）A，α = 73.573（1）度，β = 78.632（1）度，伽马= 89.621（1）度，V = 4129.1（1）A（3），Z = 4（两个独立分子），三斜晶系，空间群P（-）1，R1（所有数据）= 0.0902; Sr[NDiip（SiMe（3））]（2）THF（2），5，a = 20.5874（5）A，B = 9.8785（2）A，c = 20.8522（5）A，β = 102.035（2）度，V = 4147.6（2）A（3），Z = 4（两个独立分子），单斜晶系，空间群P2/n，R1（所有数据）= 0.0756; Ba[NDiip（SiMe（3））]（2）THF（2），6，a = 20.5476（2）A，B = 10.0353（2）A，c = 20.9020（4）A，β = 101.657（1）度，V = 4221.0（1）A（3），Z = 4（两个独立分子），单斜晶系，空间群P2/n，R1（所有数据）= 0.0573。
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(SiMe(3)), (Diip = 2,6-i-Pr(2)C(6)H(3)). The organomagnesium source for the alkane elimination was ((n)()Bu/(s)()Bu)(2)Mg. All compounds were characterized using (1)H, (13)C NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDiip(SiMe(3))](2)THF(2)). Crystal data with Mo Kalpha (lambda = 0.710 73 A) are as follows: Mg[NDiip(SiMe(3))](2), 1, a = 9.4687(6) A, b = 9.6818(6) A, c = 17.9296(1) A, alpha = 96.487(1) degrees, beta = 94.537(1) degrees, gamma = 89.222(1) degrees, V = 1608.8(2) A(3), Z = 2 (two independent molecules), triclinic, space group P(-)1, R1 (all data) = 0.0508; (n)()BuMg[NDiip(SiMe(3))]THF(2), 2, a = 9.5413(1) A, b = 16.493(2) A, c = 9.8218(1) A, beta = 108.149(2) degrees, V = 1468.7(4) A(3), Z = 2, monoclinic, space group P2(1), R1(all data) = 0.1232; Ca[NDiip(SiMe(3))](2)THF(2), 4, a = 9.7074(1) A, b = 20.9466(4) A, c = 21.6242(3) A, alpha = 73.573(1) degrees, beta = 78.632(1) degrees, gamma = 89.621(1) degrees, V = 4129.1(1) A(3), Z = 4 (two independent molecules), triclinic, space group P(-)1, R1 (all data) = 0.0902; Sr[NDiip(SiMe(3))](2)THF(2), 5, a = 20.5874(5) A, b = 9.8785(2) A, c = 20.8522(5) A, beta = 102.035(2) degrees, V = 4147.6(2) A(3), Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0756; Ba[NDiip(SiMe(3))](2)THF(2), 6, a = 20.5476(2) A, b = 10.0353(2) A, c = 20.9020(4) A, beta = 101.657(1) degrees, V = 4221.0(1) A(3), Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.