Experiment 3.8 NMR Spectroscopic Analysis of

This experiment incorporates advanced theory and data analysis. In this experiment, you will use one- and two-dimensional NMR spectroscopy to investigate the solution structure of the brown [Ni(salpd)] complex. A brief introduction to pulsed NMR spectroscopy is given Appendix 1. 

For systems that exhibit contact shifts in solution, the total spin density, p, centered on the s orbital of the shifted nucleus, i, is equal to the number of unpaired electrons on the paramagnetic center, equation (3.30). The value for pt for each resonance is 

The value for A, is the difference in chemical shift of the ligand resonance bound to nickel(II) and bound to an analogous diamagnetic probe [e.g., zinc(II)]. 

Place 50 mg salpd ligand in 1 ml CDCI3 containing a reference (e.g., TMS). In another tube, place 30 mg salpd ligand in 1 ml Jg-DMSO containing a reference (e.g., DSS). 

Place 50 mg brown [Ni(salpd)] complex in 1 ml CDC13 with reference and in another tube, place 10mg (amount is limited by solubility) in 1 ml 76-DMSO with a reference. 

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