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同配型双（1,4 - 二叔丁基 - 1,4 - 二氮杂 - 1,3 - 丁二烯）锌配合物的同系物：K(x)[Zn(t - BuNCHCHN - t - Bu)(2)]、Zn(t - BuNCHCHN - t - Bu)(2)和[Zn(t - BuNCHCHN - t - Bu)(2)](OTf)(x)（x = 1, 2）

A Homologous Series of Homoleptic Zinc Bis(1,4-di-tert-butyl-1,4-diaza-1,3-butadiene) Complexes: K(x)[Zn(t-BuNCHCHN-t-Bu)(2)], Zn(t-BuNCHCHN-t-Bu)(2), and [Zn(t-BuNCHCHN-t-Bu)(2)](OTf)(x) (x = 1, 2).

作者信息

Rijnberg Evelien, Richter Bodo, Thiele Karl-H., Boersma Jaap, Veldman Nora, Spek Anthony L., van Koten Gerard

机构信息

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.

出版信息

Inorg Chem. 1998 Jan 12;37(1):56-63. doi: 10.1021/ic970698q.

DOI:10.1021/ic970698q
PMID:11670260
Abstract

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.

摘要

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.

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