2
This work by Dr. James S. Nowick, Professor of Chemistry, University of California, Irvine, is licensed under a Creative Commons Attribution 4.0 International License.
1. The following spectral data are provided for a tricyclic compound: 500.22 MHz 1
H NMR, 125.79
MHz 13
C NMR, DEPT, COSY, TOCSY, HMQC, HMBC, NOESY, and HSQC-TOCSY spectra with 5-,
10-, 20-, and 100-ms mixing times. All NMR spectra were measured in C6D6 solution.
O
CH3H3C
H
CH3
CH3
H
Using these data, determine the stereochemistry and assign all of the 1
H and 13
C resonances to their
respective atoms in the structure. Specifically, assign the stereochemistry of the two stereocenters shown
with squiggly lines, and hence which of the four possible diastereomers (1, 2, 3, or 4) is consistent with
these data.
O
CH3H3C
H
CH3
CH3
H
1
O
CH3H3C
H
CH3
CH3
H
2
O
CH3H3C
H
CH3
CH3
H
3
O
CH3H3C
H
CH3
CH3
H
4
MAKE SURE TO COMPLETELY ANSWER THE QUESTIONS a-g ON PAGES 2-6.
1234567ppm
Integral
2.0000
1.0055
5.0773
3.9746
5.0708
7.9270
2.9365
ppm
7.16283
3.89098
3.87533
3.86530
3.85018
3.83438
3.81861
3.80276
3.78579
2.00062
1.97573
1.58401
1.55626
1.53778
1.51217
1.48849
1.47237
1.46323
1.45039
1.43535
1.34952
1.32423
1.30676
1.28301
1.15622
1.12625
1.09978
1.05830
0.85683
0.83577
0.81240
0.77946
0.70195
0.64099
1H spectrum at 500 MHz in C6D6
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 2
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111128
Time 11.59
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
zg30
TD 81728
SOLVENT C6D6
NS 8
DS 2
SWH 8012.820 Hz
FIDRES 0.098043 Hz
AQ 5.0998774 sec
RG 7.1
DW 62.400 usec
DE 6.00 usec
TE 298.0 K
D1 0.10000000 sec
MCREST 0.00000000 sec
MCWRK 0.01500000 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
PL1 1.60 dB
SFO1 500.2235015 MHz
F2 - Processing parameters
SI 65536
SF 500.2200000 MHz
WDW no
SSB 0
LB 0.00 Hz
GB 0
PC 4.00
1D NMR plot parameters
CX 22.80 cm
CY 15.00 cm
F1P 8.000 ppm
F1 4001.76 Hz
F2P 0.000 ppm
F2 0.00 Hz
PPMCM 0.35088 ppm/cm
HZCM 175.51579 Hz/cm
C D H
DU=/v, USER=nmr11t, NAME=nmr-X-sample11, EXPNO=2, PROCNO=1
F1=4.200ppm, F2=0.500ppm, MI=0.50cm, MAXI=10000.00cm, PC=4.000
# ADDRESS FREQUENCY INTENSITY
[Hz] [PPM]
1 45487.8 1946.347 3.8910 0.62
2 45551.8 1938.519 3.8753 1.37
3 45592.8 1933.502 3.8653 1.56
4 45654.7 1925.939 3.8502 0.99
5 45719.3 1918.036 3.8344 1.01
6 45783.9 1910.146 3.8186 2.35
7 45848.7 1902.217 3.8028 1.94
8 45918.1 1893.729 3.7858 0.58
9 53221.7 1000.748 2.0006 1.60
10 53323.6 988.298 1.9757 1.43
11 54926.2 792.353 1.5840 1.52
12 55039.7 778.472 1.5563 2.64
13 55115.3 769.226 1.5378 2.07
14 55220.1 756.417 1.5122 0.87
15 55317.0 744.573 1.4885 0.68
16 55382.9 736.512 1.4724 1.71
17 55420.3 731.938 1.4632 2.20
18 55472.8 725.515 1.4504 2.86
19 55534.3 717.993 1.4354 1.65
20 55885.5 675.057 1.3495 2.09
21 55989.0 662.406 1.3242 3.36
22 56060.4 653.669 1.3068 2.86
23 56157.6 641.786 1.2830 1.99
24 56676.4 578.362 1.1562 0.61
25 56799.0 563.371 1.1262 1.70
26 56907.3 550.131 1.0998 2.12
27 57077.0 529.382 1.0583 13.83
28 57901.2 428.605 0.8568 0.86
29 57987.4 418.071 0.8358 1.69
30 58083.0 406.376 0.8124 15.00
31 58217.8 389.900 0.7795 13.22
32 58534.9 351.131 0.7020 13.21
33 58784.3 320.638 0.6410 1.03
1.01.52.02.53.03.54.0ppm
Integral
2.0000
1.0055
5.0773
3.9746
5.0708
7.9270
2.9365
ppm
3.89098
3.87533
3.86530
3.85018
3.83438
3.81861
3.80276
3.78579
2.00062
1.97573
1.58401
1.55626
1.53778
1.51217
1.48849
1.47237
1.46323
1.45039
1.43535
1.34952
1.32423
1.30676
1.28301
1.15622
1.12625
1.09978
1.05830
0.85683
0.83577
0.81240
0.77946
0.70195
0.64099
1H spectrum at 500 MHz in C D
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 2
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111128
Time 11.59
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
zg30
TD 81728
SOLVENT C6D6
NS 8
DS 2
SWH 8012.820 Hz
FIDRES 0.098043 Hz
AQ 5.0998774 sec
RG 7.1
DW 62.400 usec
DE 6.00 usec
TE 298.0 K
D1 0.10000000 sec
MCREST 0.00000000 sec
MCWRK 0.01500000 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
PL1 1.60 dB
SFO1 500.2235015 MHz
F2 - Processing parameters
SI 65536
SF 500.2200000 MHz
WDW no
SSB 0
LB 0.00 Hz
GB 0
PC 4.00
1D NMR plot parameters
CX 22.80 cm
CY 15.00 cm
F1P 4.200 ppm
F1 2100.92 Hz
F2P 0.500 ppm
F2 250.11 Hz
PPMCM 0.16228 ppm/cm
HZCM 81.17605 Hz/cm
a b
c
d
e f
g
h
i
j
k l
20406080100120140ppm
ppm
128.00
127.90
127.81
127.71
127.62
127.52
79.41
64.65
60.19
57.00
42.37
40.06
39.74
35.97
33.39
32.82
22.57
21.15
20.96
20.61
18.45
14.85
Z-restored spin-echo 13C spectrum with 1H decoupling at 125 MHz in C6D6
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 3
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111128
Time 12.02
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
SpinEchopg30gp.prd
TD 65536
SOLVENT C6D6
NS 330
DS 16
SWH 30303.031 Hz
FIDRES 0.462388 Hz
AQ 1.0813940 sec
RG 32768
DW 16.500 usec
DE 6.00 usec
TE 298.0 K
D1 0.25000000 sec
d11 0.03000000 sec
D16 0.00020000 sec
d17 0.00019600 sec
MCREST 0.00000000 sec
MCWRK 0.01500000 sec
P2 31.00 usec
======== CHANNEL f1 ========
NUC1 13C
P1 15.50 usec
P11 500.00 usec
P12 2000.00 usec
PL0 120.00 dB
PL1 -1.00 dB
SFO1 125.7942548 MHz
SP1 3.20 dB
SP2 3.20 dB
SPNAM1 Crp60,0.5,20.1
SPNAM2 Crp60comp.4
SPOFF1 0.00 Hz
SPOFF2 0.00 Hz
======== CHANNEL f2 ========
CPDPRG2 waltz16
NUC2 1H
PCPD2 100.00 usec
PL2 1.60 dB
PL12 24.60 dB
SFO2 500.2225011 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 30.00 %
GPZ2 50.00 %
p15 500.00 usec
p16 1000.00 usec
F2 - Processing parameters
SI 65536
SF 125.7804190 MHz
WDW EM
SSB 0
LB 1.00 Hz
GB 0
PC 2.00
1D NMR plot parameters
CX 22.80 cm
CY 15.65 cm
F1P 160.000 ppm
F1 20124.87 Hz
F2P 0.000 ppm
F2 0.00 Hz
PPMCM 7.01754 ppm/cm
HZCM 882.66962 Hz/cm
C D
1020304050607080ppm
ppm
79.407
64.654
60.189
57.002
42.374
40.058
39.738
35.970
33.387
32.819
22.568
21.149
20.963
20.609
18.448
14.849
Z-restored spin-echo 13C spectrum with 1H decoupling at 125 MHz in C D
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 3
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111128
Time 12.02
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
SpinEchopg30gp.prd
TD 65536
SOLVENT C6D6
NS 330
DS 16
SWH 30303.031 Hz
FIDRES 0.462388 Hz
AQ 1.0813940 sec
RG 32768
DW 16.500 usec
DE 6.00 usec
TE 298.0 K
D1 0.25000000 sec
d11 0.03000000 sec
D16 0.00020000 sec
d17 0.00019600 sec
MCREST 0.00000000 sec
MCWRK 0.01500000 sec
P2 31.00 usec
======== CHANNEL f1 ========
NUC1 13C
P1 15.50 usec
P11 500.00 usec
P12 2000.00 usec
PL0 120.00 dB
PL1 -1.00 dB
SFO1 125.7942548 MHz
SP1 3.20 dB
SP2 3.20 dB
SPNAM1 Crp60,0.5,20.1
SPNAM2 Crp60comp.4
SPOFF1 0.00 Hz
SPOFF2 0.00 Hz
======== CHANNEL f2 ========
CPDPRG2 waltz16
NUC2 1H
PCPD2 100.00 usec
PL2 1.60 dB
PL12 24.60 dB
SFO2 500.2225011 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 30.00 %
GPZ2 50.00 %
p15 500.00 usec
p16 1000.00 usec
F2 - Processing parameters
SI 65536
SF 125.7804190 MHz
WDW EM
SSB 0
LB 1.00 Hz
GB 0
PC 2.00
1D NMR plot parameters
CX 22.80 cm
CY 15.65 cm
F1P 90.000 ppm
F1 11320.24 Hz
F2P 0.000 ppm
F2 0.00 Hz
PPMCM 3.94737 ppm/cm
HZCM 496.50168 Hz/cm
1
2
3 4
5 6
7
8
9
10
11
12, 13
14 15
16
1020304050607080ppm
ppm
79.407
64.654
60.189
57.002
42.373
40.058
39.738
35.969
33.387
32.818
22.567
21.149
20.962
20.608
18.448
14.849
Z-restored spin-echo 13C spectrum with 1H decoupling at 125 MHz in C6D6
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 5
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111128
Time 12.02
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
SpinEchopg30gp.prd
TD 65536
SOLVENT CDCl3
NS 330
DS 16
SWH 30303.031 Hz
FIDRES 0.462388 Hz
AQ 1.0813940 sec
RG 32768
DW 16.500 usec
DE 6.00 usec
TE 298.0 K
D1 0.25000000 sec
d11 0.03000000 sec
D16 0.00020000 sec
d17 0.00019600 sec
MCREST 0.00000000 sec
MCWRK 0.01500000 sec
P2 31.00 usec
======== CHANNEL f1 ========
NUC1 13C
P1 15.50 usec
P11 500.00 usec
P12 2000.00 usec
PL0 120.00 dB
PL1 -1.00 dB
SFO1 125.7942548 MHz
SP1 3.20 dB
SP2 3.20 dB
SPNAM1 Crp60,0.5,20.1
SPNAM2 Crp60comp.4
SPOFF1 0.00 Hz
SPOFF2 0.00 Hz
======== CHANNEL f2 ========
CPDPRG2 waltz16
NUC2 1H
PCPD2 100.00 usec
PL2 1.60 dB
PL12 24.60 dB
SFO2 500.2225011 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 30.00 %
GPZ2 50.00 %
p15 500.00 usec
p16 1000.00 usec
F2 - Processing parameters
SI 65536
SF 125.7804190 MHz
WDW EM
SSB 0
LB 1.00 Hz
GB 0
PC 2.00
1D NMR plot parameters
CX 22.80 cm
CY 3.56 cm
F1P 90.000 ppm
F1 11320.24 Hz
F2P 0.000 ppm
F2 0.00 Hz
PPMCM 3.94737 ppm/cm
HZCM 496.50168 Hz/cm
13C{1H}
dept135
dept90
1
2
3
4
ppm
1234ppm
gcosy60
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 8
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111130
Time 21.35
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
cosygp60.prd
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 35.9
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
d0 0.00000300 sec
D1 1.00000000 sec
d13 0.00000300 sec
D16 0.00020000 sec
IN0 0.00048000 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 17.00 %
GPZ2 17.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 1
TD 512
SFO1 500.2211 MHz
FIDRES 4.069010 Hz
SW 4.165 ppm
FnMODE undefined
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
PC 1.00
F1 - Processing parameters
SI 1024
MC2 QF
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 15.00 cm
CX1 15.00 cm
F2PLO 4.326 ppm
F2LO 2164.12 Hz
F2PHI 0.162 ppm
F2HI 80.79 Hz
F1PLO 4.326 ppm
F1LO 2164.12 Hz
F1PHI 0.162 ppm
F1HI 80.79 Hz
F2PPMCM 0.27766 ppm/cm
F2HZCM 138.88889 Hz/cm
F1PPMCM 0.27766 ppm/cm
F1HZCM 138.88889 Hz/cm
1
2
3
4
ppm
1234ppm
gtocsy
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 9
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111130
Time 22.32
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
mlevgp_mo
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 35.9
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
d0 0.00000300 sec
D1 2.00000000 sec
D9 0.06000000 sec
d12 0.00002000 sec
D16 0.00020000 sec
FACTOR1 4
IN0 0.00048000 sec
l1 24
SCALEF 6
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p5 23.34 usec
P6 35.00 usec
p7 70.00 usec
P17 2500.00 usec
PL1 1.60 dB
PL10 15.20 dB
SFO1 500.2211225 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 10.00 %
GPZ2 10.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 1
TD 512
SFO1 500.2211 MHz
FIDRES 4.069010 Hz
SW 4.165 ppm
FnMODE undefined
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 QF
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 15.00 cm
CX1 15.00 cm
F2PLO 4.326 ppm
F2LO 2164.12 Hz
F2PHI 0.162 ppm
F2HI 80.79 Hz
F1PLO 4.326 ppm
F1LO 2164.12 Hz
F1PHI 0.162 ppm
F1HI 80.79 Hz
F2PPMCM 0.27766 ppm/cm
F2HZCM 138.88889 Hz/cm
F1PPMCM 0.27766 ppm/cm
F1HZCM 138.88889 Hz/cm
20
30
40
50
60
ppm
0.51.01.52.02.53.03.54.0ppm
ghmqc
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 10
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 0.04
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
inv4gp.wu
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 7298.2
DW 240.000 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 1.00000000 sec
d2 0.00344828 sec
d12 0.00002000 sec
d13 0.00000300 sec
D16 0.00020000 sec
d20 0.00242528 sec
IN0 0.00004960 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7865620 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPNAM3 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPX3 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPY3 0.00 %
GPZ1 30.00 %
GPZ2 18.00 %
GPZ3 24.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 125.7866 MHz
FIDRES 19.688761 Hz
SW 80.141 ppm
FnMODE undefined
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 QF
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.326 ppm
F2LO 2164.12 Hz
F2PHI 0.162 ppm
F2HI 80.79 Hz
F1PLO 70.000 ppm
F1LO 8804.63 Hz
F1PHI 10.000 ppm
F1HI 1257.80 Hz
F2PPMCM 0.23138 ppm/cm
F2HZCM 115.74074 Hz/cm
F1PPMCM 4.00000 ppm/cm
F1HZCM 503.12167 Hz/cm
18
20
22
24
ppm
0.51.01.5ppm
ghmqc
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 10
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 0.04
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
inv4gp.wu
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 7298.2
DW 240.000 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 1.00000000 sec
d2 0.00344828 sec
d12 0.00002000 sec
d13 0.00000300 sec
D16 0.00020000 sec
d20 0.00242528 sec
IN0 0.00004960 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7865620 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPNAM3 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPX3 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPY3 0.00 %
GPZ1 30.00 %
GPZ2 18.00 %
GPZ3 24.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 125.7866 MHz
FIDRES 19.688761 Hz
SW 80.141 ppm
FnMODE undefined
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 QF
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 2.004 ppm
F2LO 1002.42 Hz
F2PHI 0.149 ppm
F2HI 74.69 Hz
F1PLO 25.046 ppm
F1LO 3150.33 Hz
F1PHI 16.000 ppm
F1HI 2012.49 Hz
F2PPMCM 0.10304 ppm/cm
F2HZCM 51.54080 Hz/cm
F1PPMCM 0.60308 ppm/cm
F1HZCM 75.85626 Hz/cm
20
30
40
50
60
70
ppm
1.01.52.02.53.03.5ppm
ghmbc optimised for 10 Hz couplings
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 11
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 0.57
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
ghmbc.wu
TD 4096
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 0.508626 Hz
AQ 0.9830900 sec
RG 8192
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 1.25000000 sec
d2 0.00344828 sec
D6 0.05000000 sec
d13 0.00000300 sec
D16 0.00020000 sec
IN0 0.00004960 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
======== CHANNEL f2 ========
NUC2 13C
P3 15.50 usec
PL2 -1.00 dB
SFO2 125.7865620 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPNAM3 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPX3 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPY3 0.00 %
GPZ1 50.00 %
GPZ2 30.00 %
GPZ3 40.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 125.7866 MHz
FIDRES 19.688761 Hz
SW 80.141 ppm
FnMODE undefined
F2 - Processing parameters
SI 2048
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 QF
SF 125.7804190 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.001 ppm
F2LO 2001.36 Hz
F2PHI 0.499 ppm
F2HI 249.65 Hz
F1PLO 81.007 ppm
F1LO 10189.06 Hz
F1PHI 14.950 ppm
F1HI 1880.41 Hz
F2PPMCM 0.19455 ppm/cm
F2HZCM 97.31716 Hz/cm
F1PPMCM 4.40379 ppm/cm
F1HZCM 553.91046 Hz/cm
20
30
40
50
60
70
ppm
0.70.80.91.01.1ppm
ghmbc optimised for 10 Hz couplings
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 11
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 0.57
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
ghmbc.wu
TD 4096
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 0.508626 Hz
AQ 0.9830900 sec
RG 8192
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 1.25000000 sec
d2 0.00344828 sec
D6 0.05000000 sec
d13 0.00000300 sec
D16 0.00020000 sec
IN0 0.00004960 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
======== CHANNEL f2 ========
NUC2 13C
P3 15.50 usec
PL2 -1.00 dB
SFO2 125.7865620 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPNAM3 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPX3 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPY3 0.00 %
GPZ1 50.00 %
GPZ2 30.00 %
GPZ3 40.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 125.7866 MHz
FIDRES 19.688761 Hz
SW 80.141 ppm
FnMODE undefined
F2 - Processing parameters
SI 2048
SF 500.2200000 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 QF
SF 125.7804190 MHz
WDW SINE
SSB 0
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 1.201 ppm
F2LO 600.61 Hz
F2PHI 0.599 ppm
F2HI 299.50 Hz
F1PLO 81.000 ppm
F1LO 10188.21 Hz
F1PHI 14.950 ppm
F1HI 1880.41 Hz
F2PPMCM 0.03344 ppm/cm
F2HZCM 16.72815 Hz/cm
F1PPMCM 4.40334 ppm/cm
F1HZCM 553.85388 Hz/cm
1
2
3
4
ppm
1234ppm
gnoesy
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 12
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 2.17
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
noesygptp
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 25.4
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
D0 0.00000300 sec
D1 2.00000000 sec
D8 0.80000001 sec
D16 0.00020000 sec
d20 0.39880002 sec
IN0 0.00024000 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
P2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 40.00 %
GPZ2 -40.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 500.2211 MHz
FIDRES 4.069010 Hz
SW 4.165 ppm
FnMODE undefined
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW QSINE
SSB 2
LB 0.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 TPPI
SF 500.2200000 MHz
WDW QSINE
SSB 2
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 15.00 cm
CX1 15.00 cm
F2PLO 4.326 ppm
F2LO 2164.12 Hz
F2PHI 0.162 ppm
F2HI 80.79 Hz
F1PLO 4.326 ppm
F1LO 2164.12 Hz
F1PHI 0.162 ppm
F1HI 80.79 Hz
F2PPMCM 0.27766 ppm/cm
F2HZCM 138.88889 Hz/cm
F1PPMCM 0.27766 ppm/cm
F1HZCM 138.88889 Hz/cm
0.8
1.0
1.2
1.4
1.6
ppm
0.81.01.21.41.6ppm
gnoesy
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 12
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111201
Time 2.17
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
noesygptp
TD 2048
SOLVENT CDCl3
NS 4
DS 16
SWH 2083.333 Hz
FIDRES 1.017253 Hz
AQ 0.4915700 sec
RG 25.4
DW 240.000 usec
DE 6.00 usec
TE 298.0 K
D0 0.00000300 sec
D1 2.00000000 sec
D8 0.80000001 sec
D16 0.00020000 sec
d20 0.39880002 sec
IN0 0.00024000 sec
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
P2 15.00 usec
PL1 1.60 dB
SFO1 500.2211225 MHz
====== GRADIENT CHANNEL =====
GPNAM1 sine.100
GPNAM2 sine.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 40.00 %
GPZ2 -40.00 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 512
SFO1 500.2211 MHz
FIDRES 4.069010 Hz
SW 4.165 ppm
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW QSINE
SSB 2
LB 0.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 TPPI
SF 500.2200000 MHz
WDW QSINE
SSB 2
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 15.00 cm
CX1 15.00 cm
F2PLO 1.700 ppm
F2LO 850.37 Hz
F2PHI 0.597 ppm
F2HI 298.48 Hz
F1PLO 1.700 ppm
F1LO 850.37 Hz
F1PHI 0.593 ppm
F1HI 296.45 Hz
F2PPMCM 0.07355 ppm/cm
F2HZCM 36.79276 Hz/cm
F1PPMCM 0.07382 ppm/cm
F1HZCM 36.92840 Hz/cm
20
30
40
50
60
ppm
0.51.01.52.02.53.03.54.0ppm
HSQC-TOCSY (hsqcetgpml) 5ms
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 18
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111206
Time 21.27
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
hsqcetgpml
TD 2048
SOLVENT C6D6
NS 4
DS 32
SWH 2248.201 Hz
FIDRES 1.097755 Hz
AQ 0.4555252 sec
RG 5160.6
DW 222.400 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 2.00000000 sec
d4 0.00172414 sec
D9 0.00500000 sec
d11 0.03000000 sec
d12 0.00002000 sec
d13 0.00000400 sec
D16 0.00020000 sec
DELTA 0.00122100 sec
DELTA1 0.00120800 sec
FACTOR1 0
IN0 0.00004680 sec
l1 0
MCREST 0.00000000 sec
MCWRK 0.40000001 sec
SCALEF 6
ST1CNT 256
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
p5 23.34 usec
P6 35.00 usec
p7 70.00 usec
P17 2500.00 usec
P28 1000.00 usec
PL1 1.60 dB
PL10 15.20 dB
SFO1 500.2211251 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
p4 31.00 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7863936 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 80.00 %
GPZ2 20.10 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 1024
SFO1 125.7864 MHz
FIDRES 10.433360 Hz
SW 84.936 ppm
FnMODE Echo-Antiecho
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.00
F1 - Processing parameters
SI 1024
MC2 echo-antiecho
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.496 ppm
F2LO 2249.15 Hz
F2PHI 0.002 ppm
F2HI 0.95 Hz
F1PLO 70.000 ppm
F1LO 8804.63 Hz
F1PHI 10.000 ppm
F1HI 1257.80 Hz
F2PPMCM 0.24969 ppm/cm
F2HZCM 124.90008 Hz/cm
F1PPMCM 4.00000 ppm/cm
F1HZCM 503.12167 Hz/cm
20
30
40
50
60
ppm
0.51.01.52.02.53.03.54.0ppm
HSQC-TOCSY 10 ms
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 19
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111207
Time 0.19
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
hsqcetgpml
TD 2048
SOLVENT C6D6
NS 4
DS 32
SWH 2248.201 Hz
FIDRES 1.097755 Hz
AQ 0.4555252 sec
RG 4597.6
DW 222.400 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 2.00000000 sec
d4 0.00172414 sec
D9 0.01000000 sec
d11 0.03000000 sec
d12 0.00002000 sec
d13 0.00000400 sec
D16 0.00020000 sec
DELTA 0.00122100 sec
DELTA1 0.00120800 sec
FACTOR1 0
IN0 0.00004680 sec
l1 0
MCREST 0.00000000 sec
MCWRK 0.40000001 sec
SCALEF 6
ST1CNT 256
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
p5 23.34 usec
P6 35.00 usec
p7 70.00 usec
P17 2500.00 usec
P28 1000.00 usec
PL1 1.60 dB
PL10 15.20 dB
SFO1 500.2211251 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
p4 31.00 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7863936 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 80.00 %
GPZ2 20.10 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 1024
SFO1 125.7864 MHz
FIDRES 10.433360 Hz
SW 84.936 ppm
FnMODE Echo-Antiecho
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 echo-antiecho
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.496 ppm
F2LO 2249.15 Hz
F2PHI 0.002 ppm
F2HI 0.95 Hz
F1PLO 70.000 ppm
F1LO 8804.63 Hz
F1PHI 10.000 ppm
F1HI 1257.80 Hz
F2PPMCM 0.24969 ppm/cm
F2HZCM 124.90008 Hz/cm
F1PPMCM 4.00000 ppm/cm
F1HZCM 503.12167 Hz/cm
20
30
40
50
60
ppm
0.51.01.52.02.53.03.54.0ppm
HSQC-TOCSY 20 ms
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 20
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111207
Time 3.11
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
hsqcetgpml
TD 2048
SOLVENT C6D6
NS 4
DS 32
SWH 2248.201 Hz
FIDRES 1.097755 Hz
AQ 0.4555252 sec
RG 4096
DW 222.400 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 2.00000000 sec
d4 0.00172414 sec
D9 0.02000000 sec
d11 0.03000000 sec
d12 0.00002000 sec
d13 0.00000400 sec
D16 0.00020000 sec
DELTA 0.00122100 sec
DELTA1 0.00120800 sec
FACTOR1 1
IN0 0.00004680 sec
l1 6
MCREST 0.00000000 sec
MCWRK 0.40000001 sec
SCALEF 6
ST1CNT 256
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
p5 23.34 usec
P6 35.00 usec
p7 70.00 usec
P17 2500.00 usec
P28 1000.00 usec
PL1 1.60 dB
PL10 15.20 dB
SFO1 500.2211251 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
p4 31.00 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7863936 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 80.00 %
GPZ2 20.10 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 1024
SFO1 125.7864 MHz
FIDRES 10.433360 Hz
SW 84.936 ppm
FnMODE Echo-Antiecho
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 echo-antiecho
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.496 ppm
F2LO 2249.15 Hz
F2PHI 0.002 ppm
F2HI 0.95 Hz
F1PLO 70.000 ppm
F1LO 8804.63 Hz
F1PHI 10.000 ppm
F1HI 1257.80 Hz
F2PPMCM 0.24969 ppm/cm
F2HZCM 124.90008 Hz/cm
F1PPMCM 4.00000 ppm/cm
F1HZCM 503.12167 Hz/cm
20
30
40
50
60
ppm
0.51.01.52.02.53.03.54.0ppm
HSQC-TOCSY 100 ms
Current Data Parameters
USER nmr11t
NAME nmr-X-sample11
EXPNO 21
PROCNO 1
F2 - Acquisition Parameters
Date_ 20111207
Time 6.05
INSTRUM cryo500
PROBHD 5 mm CPTCI 1HPULPROG
hsqcetgpml
TD 2048
SOLVENT C6D6
NS 4
DS 32
SWH 2248.201 Hz
FIDRES 1.097755 Hz
AQ 0.4555252 sec
RG 18390.4
DW 222.400 usec
DE 6.50 usec
TE 298.0 K
CNST2 145.0000000
d0 0.00000300 sec
D1 2.00000000 sec
d4 0.00172414 sec
D9 0.10000000 sec
d11 0.03000000 sec
d12 0.00002000 sec
d13 0.00000400 sec
D16 0.00020000 sec
DELTA 0.00122100 sec
DELTA1 0.00120800 sec
FACTOR1 7
IN0 0.00004680 sec
l1 42
MCREST 0.00000000 sec
MCWRK 0.40000001 sec
SCALEF 6
ST1CNT 256
======== CHANNEL f1 ========
NUC1 1H
P1 7.50 usec
p2 15.00 usec
p5 23.34 usec
P6 35.00 usec
p7 70.00 usec
P17 2500.00 usec
P28 1000.00 usec
PL1 1.60 dB
PL10 15.20 dB
SFO1 500.2211251 MHz
======== CHANNEL f2 ========
CPDPRG2 garp
NUC2 13C
P3 15.50 usec
p4 31.00 usec
PCPD2 65.00 usec
PL2 -1.00 dB
PL12 11.30 dB
SFO2 125.7863936 MHz
====== GRADIENT CHANNEL =====
GPNAM1 SINE.100
GPNAM2 SINE.100
GPX1 0.00 %
GPX2 0.00 %
GPY1 0.00 %
GPY2 0.00 %
GPZ1 80.00 %
GPZ2 20.10 %
P16 1000.00 usec
F1 - Acquisition parameters
ND0 2
TD 1024
SFO1 125.7864 MHz
FIDRES 10.433360 Hz
SW 84.936 ppm
FnMODE Echo-Antiecho
F2 - Processing parameters
SI 1024
SF 500.2200000 MHz
WDW EM
SSB 0
LB 5.00 Hz
GB 0
PC 1.40
F1 - Processing parameters
SI 1024
MC2 echo-antiecho
SF 125.7804190 MHz
WDW QSINE
SSB 3
LB 0.00 Hz
GB 0
2D NMR plot parameters
CX2 18.00 cm
CX1 15.00 cm
F2PLO 4.496 ppm
F2LO 2249.15 Hz
F2PHI -0.002 ppm
F2HI -1.24 Hz
F1PLO 70.062 ppm
F1LO 8812.44 Hz
F1PHI 9.924 ppm
F1HI 1248.25 Hz
F2PPMCM 0.24993 ppm/cm
F2HZCM 125.02204 Hz/cm
F1PPMCM 4.00920 ppm/cm
F1HZCM 504.27905 Hz/cm