nmr lecture 3 oct.26, psc 311 zhenming (jimmy) du … · 2017. 12. 23. · 1.the absolute value...
TRANSCRIPT
![Page 2: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/2.jpg)
Q1: What is 2D NMR?
Q2: Why 2D NMR?
Q3: Which 2D NMR?
![Page 3: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/3.jpg)
![Page 4: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/4.jpg)
![Page 5: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/5.jpg)
![Page 6: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/6.jpg)
![Page 7: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/7.jpg)
![Page 8: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/8.jpg)
![Page 9: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/9.jpg)
![Page 10: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/10.jpg)
![Page 11: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/11.jpg)
![Page 12: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/12.jpg)
![Page 13: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/13.jpg)
![Page 14: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/14.jpg)
![Page 15: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/15.jpg)
1. Resolves crowed peaks
![Page 16: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/16.jpg)
2. 2nd Dimension information and correlation
![Page 17: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/17.jpg)
3. Cross‐peak information (phase, intensity…)Etc .NOESY intensity for structure determination
![Page 18: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/18.jpg)
Homonuclear Heteronuclear
COSYDQF‐COSYTOCSYNOESYROESY
INADEQUATE
HETCORHSQCHMQCHMBC
![Page 19: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/19.jpg)
![Page 20: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/20.jpg)
![Page 21: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/21.jpg)
Pro Con
SimpleEasy for set upForgiveness to pulse length error
Least information for H‐H 2DMainly used for smallmolecule assignment
![Page 22: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/22.jpg)
![Page 23: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/23.jpg)
![Page 24: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/24.jpg)
![Page 25: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/25.jpg)
Warnings:Strong spin lock power (25 μs)Sample heating
![Page 26: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/26.jpg)
![Page 27: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/27.jpg)
![Page 28: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/28.jpg)
![Page 29: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/29.jpg)
![Page 30: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/30.jpg)
![Page 31: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/31.jpg)
Spin‐lockLower power level in ROESY
![Page 32: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/32.jpg)
![Page 33: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/33.jpg)
![Page 34: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/34.jpg)
![Page 35: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/35.jpg)
![Page 36: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/36.jpg)
![Page 37: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/37.jpg)
![Page 38: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/38.jpg)
Absolute value or phase sensitive HETCOR?1.The absolute value HETCOR is easier to set up and process.
2.The phase sensitive HETCOR gives you narrower lines. You also have the choice to see the CH‐groups only or to see the CH‐and CH3 resonances positive and the CH2 resonances negative.
3.The final work‐up of the phase sensitive HETCOR requires phasing in both dimensions, which can be rather time‐consuming and difficult, but is do‐able. You need to be aware of peaks coming from incomplete cancellations, and have to neglect them in your phasing effort.
![Page 39: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/39.jpg)
HETCOR Advantages:
1.The set‐up is shorter.
2.To cancel artifacts, less scans are acquired, so overall HETCOR requires less time to run.
3.1H‐1H couplings are removed, while they are present in the normal HMQC. However, you can run a homonucleardecoupled version of the HMQC experiment to also remove those couplings.
4.Variations of the HETCOR can show only methines, or methines and methyls positive and methylenes negative. HMQC does not have these variations.
![Page 40: NMR Lecture 3 Oct.26, PSC 311 Zhenming (Jimmy) Du … · 2017. 12. 23. · 1.The absolute value HETCOR is easier to set up and process. 2.The phase sensitive HETCOR gives you narrower](https://reader036.vdocuments.us/reader036/viewer/2022071213/603e171a476def37d527714a/html5/thumbnails/40.jpg)
HMQC Advantages:
1.The sensitivity is 2 to 4 times greater than HETCOR for small molecules, 4 times for large molecules.
2.The 1H dimension is the "high resolution" dimension; while in HETCOR this is the 13C dimension. Typically, 1H chemical shifts span only ~10ppm, while 13C chemical shifts span ~200ppm and are normally well resolved anyway. It is therefore advantageous for the 1H dimension to have high resolution.