Varian Unity instrument

Elemental analyses were performed on a LECO CHNS 932 instrument. H-NMR spectra were determined with a Varian UNITY INOVA 500 MHz NMR spectrometer. IR spectra were recorded as KBr disks in the range of400 000 cm" on a SHIMADZU FTIR-8300 spectrometer. The electronic absorptions spectra were measiued in DMSO for 3,4 with a UNICAM UV2-100 UVATSIBLE spectrometer. 

Fig. 3. 2Q-HoMQC spectrum of apo-cytochrome c in 93% H2O at pH = 6 and 0.48 mM concentration. The spectrum was acquired with 30 ms 2Q excitation delay overnight on a Varian Unity/INOVA 600 MHz instrument using gradient MQ selection and no additional water suppression (I.P., unpublished). Equal spectral windows were set for both dimensions.

Figure 3 presents an example of such a situation. The 2Q-HoMQC spectrum of apo-cytochrome c was acquired in 93% H2O at 480 ixM concentration on a Varian Unity/INOVA 600 MHz NMR instrument overnight, using a pulse sequence with gradient coherence selection and weak gradient spin-echo during excitation delays and the evolution period [29], respectively (I.P., not published). The spectral windows were 8 kHz both in F2 and F. ... 

A Varian Unity Inova 600-MHz NMR instrument (Palo Alto, CA) equipped with a H C/ N pulse field gradient triple resonance microliow NMR probe (flow cell 60pL 3mm O.D.) was used. Reversed-phase HPLC of the samples was carried out on a Varian modular HPLC system (a 9012 pump and a 9065 photodiode array UV detector). The Varian HPLC software was also equipped with the capability for programmable stop-flow experiments based on UV peak detection. An LCQ classic MS instrument, mentioned in the previous section, was connected on-line to the HPLC-UV system of the LC-NMR by contact closure. The H resonance of the D2O was used for field-frequency lock, and the spectra were centered on the ACN methyl resonance. Suppression of resonances from HOD and methyl of ACN and its two C satellites was accomplished using a train of four selective WET pulses, each followed by a Bo gradient pulse and a composite 90-degree read pulse [41]. 

For non-deuterated complexes, NMR experiments were performed on either Vaiian Unity600 or Varian Unity+500 spectrometers. The 600 MHz instrument was equipped with a triple resonance probe and a PTS synthesizer as a pseudo fourth channel. The 500 MHz spectrometer was a four channel instrument with a triple resonance probe with an actively shielded pulsed field gradient coil. All experiments were performed at 37 C. The heteronuclear experiments shown in Figure 1 were performed as described in Zhang et al (11) and Revington et al (24). For all 3D ex riments 32 transients were required for sufficient signal to noise. This necessitated the use of fewer increments and the use of linear prediction (25)... 

The 300 MHz spectrum of pergolide mesylate (10 mg/mL) in dimethylsulfoxide-d6 (2.5 ppm) is shown in Figure 3. The spectrum was obtained on a Varian Unity spectrometer using die following instrumental parameters 5 mm jual probe spectral width, 4416 Hz 90 pulse 64K time-domain data points acquisition time, 7.421 seconds 100 scans and probe temperature, 35°C. The spectrum was provided with 0.1 Hz Lorentzian line broadening. 

General [a]o were measured with a Perkin-Elmer 241 MC polarimeter. NMR spectra of 1 were obtained on Varian VXR 200 and Varian Unity 500 spectrometers. NMR spectra of 2-5 were obtained on a Jeol JNM-LA 600 spectrometer. Chemical shifts were reported in S (ppm), with residual C3D3N signals (7.24/123.5) and CDCI3 signals (7.25/77.0) as internal standards. A Nalorac inverse probe of 5 mm was used for all NMR experiments on 2-5 except for C NMR measurements (Joel probe). D/CI mass spectra were recorded on a Finnigan MAT TSQ 700 instrument. P-Glucosidase from almonds (1000 lU/mg) was purchased from Fluka AG (No. 49290). 

A Varian Unity Inova 600 MHz NMR instrument (Palo Alto, CA), equipped with a H C/ N pulse field gradient triple resonance microflow NMR probe (flow cell 60 pL 3 mm O.D.), was used. Reverse-phase HPLC of the samples was carried out with a Varian modular HPLC system (a 9012 pump and a 9065 photodiode array UV detector). The Varian HPLC software was also... 

The H NMR spectra were recorded using a Varian Unity Inova-300 instrument. The H chemical shifts are reported in 8 units (ppm) relative to tetramethylsilane (TMS) at the external standard (8 = 0.00). 

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