4.7 Article

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

Journal

INORGANIC CHEMISTRY
Volume 41, Issue 21, Pages 5602-5608

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/ic0203668

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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 = 2,64-Pr2C6H3). The organomagnesium source for the alkane elimination was (Bu-n/Bu-s)(2)Mg. All compounds were characterized using H-1, C-13 NMR, and IR spectroscopy, in addition to X-ray crystallography (except Mg[NDiip(SiMe3)](2)THF2). Crystal data with Mo Kalpha (lambda = 0.710 73 Angstrom) are as follows: Mg[NDiip(SiMe3)](2), 1, a = 9.4687(6) Angstrom, b = 9.6818(6) Angstrom, c = 17.9296(1) Angstrom, alpha = 96.487(1)degrees, beta = 94.537(1)degrees, gamma = 89,222(1)degrees, V = 1608.8(2) Angstrom(3), Z = 2 (two independent molecules), triclinic, space group P (1) over bar, R1 (all data) = 0.0508; (BuMg)-Bu-n[NDiip(SiMe3)]THF2, 2, a = 9.5413(1) Angstrom, b = 16.493(2) Angstrom, c = 9.8218(1) Angstrom, beta = 108.149(2)degrees, V = 1468.7(4) Angstrom(3), Z = 2, monoclinic, space group P2(1), R1 (all data) = 0. 1232; Ca[NDiip(SiMe3)](2)THF2, 4, a = 9.7074(1) Angstrom, b = 20.9466(4) Angstrom, c = 21.6242(3) Angstrom, alpha = 73.573(1)degrees, beta = 78.632(1)degrees, gamma = 89.621 (1)degrees, V = 4129.1(1) Angstrom(3), Z = 4 (two independent molecules), triclinic, space group P (1) over bar, R1 (all data) = 0.0902; Sr[NDiip(SiMe3)](2)THF2, 5, a = 20.5874(5) Angstrom, b = 9.8785(2) Angstrom, c = 20.8522(5) Angstrom, beta = 102-035(2)degrees, V = 4147.6(2) Angstrom(3), Z = 4 (two independent molecules), monoclinic, space group P2ln, R1 (all data) = 0.0756; Ba[NDiip(SiMe3)](2)THF2, 6, a = 20.5476(2) Angstrom, b = 10.0353(2) Angstrom, c = 20.9020(4) Angstrom, beta = 101.657(1)degrees, V = 4221.0(1) Angstrom(3), Z = 4 (two independent molecules), monoclinic, space group P2/n, R1 (all data) = 0.0573.

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