TOCL_TMA

This dataset contains NMR spectra obtained for the sample -TOCL_TMA Nucleus: 13C NMR Solvent: H2O+D2O NMR Probe: H8609_0043 (PH MAS 500WB BL4 X/Y/H DVT) NMR Pulse Sequence: null Temperature: 295.9956 Observed Frequency: 125.78746 Magnetic Field Strength: 11.747332789100614 Number of Scans: 2048 NMR Pulse Sequence: NEA_ineptrd Spectral Width: 180.666405933068 Number of Data Points: 2270 Relaxation Delay: 6 Observed Frequency: 125.7968940595 Nucleus: 1H NMR Solvent: H2O+D2O NMR Probe: H8609_0043 (PH MAS 500WB BL4 X/Y/H DVT) NMR Pulse Sequence: null Temperature: 295.9966 Observed Frequency: 500.248 Magnetic Field Strength: 11.749122218330188 Number of Scans: 2 NMR Pulse Sequence: onepulse Spectral Width: 19.9900085939046 Number of Data Points: 3006 Relaxation Delay: 5 Observed Frequency: 500.24991 Nucleus: 31P NMR Solvent: H2O+D2O NMR Probe: H8609_0043 (PH MAS 500WB BL4 X/Y/H DVT) NMR Pulse Sequence: 1d Temperature: 295.9891 Observed Frequency: 202.504102 Magnetic Field Strength: 11.745385617451017 Number of Scans: 256 NMR Pulse Sequence: NEA_zg30bbdec Spectral Width: 201.284167395372 Number of Data Points: 5702 Relaxation Delay: 6 Observed Frequency: 202.504102 Nucleus: 31P NMR Solvent: H2O+D2O NMR Probe: H8609_0043 (PH MAS 500WB BL4 X/Y/H DVT) NMR Pulse Sequence: 1d Temperature: 295.9946 Observed Frequency: 202.504102 Magnetic Field Strength: 11.745385617451017 Number of Scans: 1024 NMR Pulse Sequence: NEA_zg30bbdec Spectral Width: 201.284167395372 Number of Data Points: 4072 Relaxation Delay: 6 Observed Frequency: 202.504102 Nucleus: 13C,1H NMR Solvent: H2O+D2O NMR Probe: H8609_0043 (PH MAS 500WB BL4 X/Y/H DVT) NMR Pulse Sequence: null Temperature: 295.988 Observed Frequency: 125.78746,500.248 Magnetic Field Strength: 11.747332789100614 Number of Scans: 256 NMR Pulse Sequence: NEA_RPDLF Spectral Width: 180.666405933068,4.99752988789391 Number of Data Points: 2270,32 Relaxation Delay: 6 Observed Frequency: 125.7968940595,500.2471333

TOCL(30.0mg,1.0 eq.) andTMACl(6.6mg,3.0eq.) weredissolvedwith2mlchloroform:methanol
(2:1, v/v) in an eppendorf vial. A solution of TMA OHx5H2O (3.6mg, 1.0eq.) and BOH3 (1.2mg,
1.0eq.) in 100µl methanol was prepared and added to the Eppendorf vial. The Folch method was
performed and 0.4ml degassed water was added to the mixture. After an immediate phase separa-
tion, the upper phase was discarded, the solvent of the lower phase was evaporated at 40°C under
a constant stream of argon and the predried sample was freeze-dried over night. 32.4µl degassed
water was added and the Eppendorf was stored at 50°C for one day. Lost water was added and
the sample was mixed thoroughly with a steel rod. After another three days of equilibration the
sample was again mixed before packing the insert.