Rijnberg Evelien, Richter Bodo, Thiele Karl-H., Boersma Jaap, Veldman Nora, Spek Anthony L., van Koten Gerard
Department of Metal-Mediated Synthesis, Debye Institute, Utrecht University, Padualaan 8, 3584 CH Utrecht, The Netherlands, Institut für Anorganische Chemie, Universität Halle, Geusaer Strasse, D-06217 Merseburg, Germany, and Bijvoet Center for Biomolecular Research and Crystal and Structural Chemistry, Utrecht University, Padualaan 8, 3584 CH Utrecht, The Netherlands.
Inorg Chem. 1998 Jan 12;37(1):56-63. doi: 10.1021/ic970698q.
A homologous series of mono- and dicationic, neutral, and mono- and dianionic zinc diazabutadiene complexes, K(x)[Zn(t-BuNCHCHN-t-Bu)(2)], Zn(t-BuNCHCHN-t-Bu)(2), and Zn(t-BuNCHCHN-t-Bu)(2)(x) (x = 1, 2), have been prepared and isolated in pure form. The crystal structures of the mono- and dicationic as well as of the monoanionic complexes are reported. In this series, the formal charge on the t-BuNCHCHN-t-Bu ligands ranges from -2 to +2, and the way in which the molecular geometry of the ligands varies with the charge is discussed. Zn(t-BuNCHCHN-t-Bu)(2)(2) reacts with methanol to give 1,3-di-tert-butylimidazolium triflate. Crystal data: dicationic 2 (Zn(t-BuNCHCHN-t-Bu)(2)(2), C(22)H(40)F(6)S(2)N(4)O(6)Zn), monoclinic, space group C2/c, with a = 18.015(6) Å, b = 9.257(6) Å, c = 20.012(5) Å, beta = 109.63(3) degrees, and Z = 4; monocationic 3.thf ([Zn(t-BuNCHCHN-t-Bu)(2)]OTf.thf, C(25)H(48)F(3)N(4)O(3)SZn), orthorhombic, space group P2(1)2(1)2(1), with a = 10.3077(6) Å, b = 17.1974(6) Å, c = 17.8241(13) Å, and Z = 4; monoanionic 5.thf (K(thf)(3)[Zn(t-BuNCHCHN-t-Bu)(2)], C(36)H(72)KN(4)O(3)Zn), triclinic, space group P&onemacr;, with a = 10.8702(10) Å, b = 11.5175(9) Å, c = 18.2815(13) Å, alpha = 73.795(6) degrees, beta = 74.227(6) degrees, gamma = 75.736(7) degrees, and Z = 2; 7 (1,3-di-tert-butylimidazolium triflate, C(12)H(21)F(3)N(2)O(3)S), orthorhombic, space group Pbca, with a = 14.4086(8) Å, b = 12.0293(8) Å, c = 18.6985(12) Å, and Z = 8.
已制备并以纯形式分离出一系列同系的单阳离子和双阳离子、中性、单阴离子和双阴离子二氮杂丁二烯锌配合物,即K(x)[Zn(t-BuNCHCHN-t-Bu)(2)]、Zn(t-BuNCHCHN-t-Bu)(2)以及Zn(t-BuNCHCHN-t-Bu)(2)(x)(x = 1, 2)。报道了单阳离子和双阳离子以及单阴离子配合物的晶体结构。在该系列中,t-BuNCHCHN-t-Bu配体上的形式电荷范围为-2至+2,并讨论了配体分子几何结构随电荷变化的方式。Zn(t-BuNCHCHN-t-Bu)(2)(2)与甲醇反应生成三氟甲磺酸1,3 - 二叔丁基咪唑鎓盐。晶体数据:双阳离子2(Zn(t-BuNCHCHN-t-Bu)(2)(2),C(22)H(40)F(6)S(2)N(4)O(6)Zn),单斜晶系,空间群C2/c,a = 18.015(6) Å,b = 9.257(6) Å,c = 20.012(5) Å,β = 109.63(3)°,Z = 4;单阳离子3·thf([Zn(t-BuNCHCHN-t-Bu)(2)]OTf·thf,C(25)H(48)F(3)N(4)O(3)SZn),正交晶系,空间群P2(1)2(1)2(1),a = 10.3077(6) Å,b = 17.1974(6) Å,c = 17.8241(13) Å,Z = 4;单阴离子5·thf(K(thf)(3)[Zn(t-BuNCHCHN-t-Bu)(2)],C(36)H(72)KN(4)O(3)Zn),三斜晶系,空间群P&onemacr;,a = 10.8702(10) Å,b = 11.5175(9) Å,c = 18.