Experimental Section & Acknowledgements
Acknowledgement of NSF Support - Instrument Purchase
"Purchase of the AVII-600 NMR spectrometer used to obtain results included in this publication was supported by the National Science Foundation under Grant No. DBI 0421374."
"Any opinions, findings, and conclusions or recommendations expressed in this material are those of the author(s) and do not necessarily reflect the views of the National Science Foundation."
Acknowledgement of CIF Staff Assistance
"We wish to thank ISU Chemical Instrumentation Facility staff members <insert name(s) here> for training and assistance pertaining to the AVII-600 results included in this publication."
Experimental Section & Publication Information
The AVII-600 NMR spectrometer features a wide bore 14.1 tesla superconducting magnet and an Avance II spectrometer console from Bruker Corporation (Billerica, MA and Karlsruhe, Germany). The spectrometer uses a BCU-Extreme for low temperature experiments. The amount of additional experimental detail necessary will depend upon whether you are?preparing a manuscript, a poster, a presentation, or including the information in your thesis.
The AVII-600 is operated using Topspin 3.0. Every data file acquired with Topspin has associated files with many of the relevant parameters from the acquisition. This data file can be accessed by opening the associated files in a text editor, or through Topspin by loading the file and typing the command?dpa<enter>.?The dpa file typically does not contain information about the temperature or MAS spinning speed at which the data was acquired.
For measurements on the AVII-600, this data file may include:
- Pulse sequence
- Number of scans (ns)
- Acquisition time (aq)
- Pulse lengths?in microseconds (typically conveted to kHz for publication - i.e. 5 us = 50 kHz pulse)
- CP contact time (typically?p15)
The spectrometer frequencies for many typical nuclei are as follows:
- ?1H = 600.13 MHz
- 31P = 242.94 MHz
- 11B = 192.55 MHz
- 13C = 150.90 MHz
- 29Si?= 119.23 MHz
- ?2H = 92.12 MHz
- 15N = 60.83 MHz
There are three probes available for the AVII-600:
- 4 mm triple resonance MAS?probe. Spinning speed is typically 5-15 kHz (15 kHz max).?
- 2.5 mm triple resonance MAS probe. Spinning speed is typically 20-35 kHz (35 kHz max).?
- 5 mm liquids four-channel?2H/13C/1H/BB?TBI probe.?