Lehrstuhl für Anorganische Chemie II, Ruhr-Universität Bochum, Universitätsstrasse 150, 44801 Bochum, Germany.
Inorg Chem. 2010 Sep 20;49(18):8487-94. doi: 10.1021/ic101060s.
The first all-nitrogen coordinated bis(alkylamidinato)/bis(alkylimido) complexes of molybdenum and tungsten, [Mo(NtBu)(2){(iPrN)(2)CMe}(2)]and [W(NtBu)(2){(iPrN)(2)CMe}(2)], have been synthesized and fully characterized by (1)H and (13)C NMR spectroscopy, elemental analyses, high-resolution electron impact mass spectrometry, and Fourier transform infrared spectroscopy. Density functional theory calculations of the tungsten complex allow for geometry optimization and structural characterization by assignment of the NMR data, in particular a comparison of the experimental (13)C NMR signals with the calculated ones. Both compounds sublime without decomposition at 130 °C and 1 mTorr and show rapid decomposition above 250 °C, hence representing promising vapor-phase deposition routes for metal nitride based thin-film materials.
首次合成并通过（1）H 和（13）C NMR 光谱、元素分析、高分辨率电子冲击质谱和傅里叶变换红外光谱对钼和钨的全氮配位双（烷基脒基）/双（烷基亚氨基）配合物[Mo（NtBu）（2）{（iPrN）（2）CMe}（2）]和[W（NtBu）（2）{（iPrN）（2）CMe}（2）]进行了全面的表征。通过计算钨配合物的密度泛函理论允许进行几何优化和结构特征的分配，特别是通过 NMR 数据的比较，尤其是实验（13）C NMR 信号与计算结果的比较。这两种化合物在 130°C 和 1 mTorr 下升华而不分解，在 250°C 以上迅速分解，因此代表了基于金属氮化物的薄膜材料的有前途的气相沉积途径。
