H(C)Ag：一种用于检测不稳定银卡宾配合物中(109)Ag的三重共振核磁共振实验。

H(C)Ag: a triple resonance NMR experiment for (109) Ag detection in labile silver-carbene complexes.

作者信息

Weske Sebastian, Li Yingjia, Wiegmann Sara, John Michael

机构信息

Georg-August-Universität, Intitut für Anorganische Chemie, Tammannstrasse 4, Göttingen, 37077, Germany.

出版信息

Magn Reson Chem. 2015 Apr;53(4):291-4. doi: 10.1002/mrc.4196. Epub 2015 Jan 12.

DOI:10.1002/mrc.4196

PMID:25641122

Abstract

In silver complexes, indirect detection of (109) Ag resonances via (1) H,(109) Ag-HMQC frequently suffers from small or absent JHAg couplings or rapid ligand dissociation. In these cases, it would be favourable to employ H(X)Ag triple resonance spectroscopy that uses the large one-bond JXAg coupling (where the donor atom of the ligand X is the relay nucleus). We have applied an HMQC-based version of the H(C)Ag experiment to a labile silver-NHC complex (NHC=N-heterocyclic carbene) at natural (13) C isotopic abundance and variable temperature. In agreement with simulations, H(C)Ag detection became superior to (1) H,(109) Ag-HMQC detection above -20 °C.

摘要

在银配合物中，通过¹H对¹⁰⁹Ag共振进行间接检测的¹H,¹⁰⁹Ag-HMQC常常受到小的或不存在的JHAg耦合或者配体快速解离的影响。在这些情况下，采用利用大的一键JXAg耦合（其中配体X的供体原子是中继核）的H(X)Ag三重共振光谱法将是有利的。我们已将基于HMQC的H(C)Ag实验应用于在天然¹³C同位素丰度和可变温度下的不稳定银-NHC配合物（NHC = N-杂环卡宾）。与模拟结果一致，在-20°C以上，H(C)Ag检测优于¹H,¹⁰⁹Ag-HMQC检测。