二水合甲酸锌的67Zn固态和单晶核磁共振光谱及X射线晶体结构

67Zn solid-state and single-crystal NMR spectroscopy and X-ray crystal structure of zinc formate dihydrate.

作者信息

Lipton Andrew S, Smith Mark D, Adams Richard D, Ellis Paul D

机构信息

Macromolecular Structure & Dynamics Directorate, WR Wiley Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland, Washington 99352, USA.

出版信息

J Am Chem Soc. 2002 Jan 23;124(3):410-4. doi: 10.1021/ja011701e.

DOI:10.1021/ja011701e

PMID:11792210

Abstract

The crystal structure, quadrupole coupling parameters, and the orientation of the electric field gradient tensors for each site of zinc formate dihydrate have been determined. There are two distinct sites in the asymmetric unit: one containing four in-plane waters with two bridging formats, the other containing six bridging formates. The solid-state NMR lineshapes have been assigned to their respective sites by using isotopic labeling and cross-polarization methods. The hydrated site corresponds to the lineshape having a quadrupole coupling constant (Cq) of 9.6 MHz and the anhydrous site has a Cq of 6.2 MHz. The absence of chemical shielding contributions to the observed lineshapes has been verified with a high-field solid-state NMR experiment performed at 18.8 T.

摘要

已确定二水合甲酸锌每个位点的晶体结构、四极耦合参数以及电场梯度张量的取向。不对称单元中有两个不同的位点：一个包含四个面内水分子和两个桥连甲酸根，另一个包含六个桥连甲酸根。通过使用同位素标记和交叉极化方法，已将固态核磁共振线形分配到它们各自的位点。水合位点对应于四极耦合常数（Cq）为9.6 MHz的线形，无水位点的Cq为6.2 MHz。在18.8 T下进行的高场固态核磁共振实验已证实，观测到的线形中不存在化学屏蔽贡献。