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© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-36p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-36pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298987 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS282p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS282pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS125p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS125pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4299002 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS172p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS172pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486778 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-41p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-41pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298992 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-48p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-48pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS278p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS278p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS292p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS292pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS294p-4
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS294p-4INOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-15p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-15p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298990 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-15p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-15p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 102 repetitionsOBSERVE C13, 125.5817522 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 1 hr, 40 min, 32 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-16p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-16p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298987 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-16p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-16p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 73 repetitionsOBSERVE C13, 125.5817512 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 20 min, 6 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-22p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-22pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298719 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-22p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-22p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 87 repetitionsOBSERVE C13, 125.5817502 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 30 min, 9 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-26p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-26p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298987 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-26p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-26p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 122 repetitionsOBSERVE C13, 125.5817483 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 40 min, 13 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-31p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-31p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4298992 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-31p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-31p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 148 repetitionsOBSERVE C13, 125.5817502 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 40 min, 13 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
STANDARD PROTON PARAMETERS
Pulse Sequence: cyclenoe5.632
4.833
4.842
4.855
4.820
3.732
3.715
1.473
1.486
ppm1.01.52.02.53.03.54.04.55.05.5
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS160p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS160pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 399.9486773 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS162p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS162pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.2 degrees Acq. time 4.665 sec Width 7024.9 Hz 8 repetitionsOBSERVE H1, 499.6964451 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 17 sec
ppm-1-01234567891011
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-38p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-38p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 145 repetitionsOBSERVE C13, 125.5817483 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 40 min, 13 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-44p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-44p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 499.4299327 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-44p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-44p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 143 repetitionsOBSERVE C13, 125.5817531 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 30 min, 9 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS223p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS223pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486778 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS223p 13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS223p-13CINOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 45.0 degrees Acq. time 1.311 sec Width 25000.0 Hz 120 repetitionsOBSERVE C13, 100.5671860 MHzDECOUPLE H1, 399.9500118 MHz Power 48 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 4 min, 38 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS181p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS181pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS224p 13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS224p-13CINOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 34.0 degrees Acq. time 1.024 sec Width 32000.0 Hz 64 repetitionsOBSERVE C13, 125.5817570 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 2 min, 10 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
STANDARD PROTON PARAMETERS
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS261pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 500.0677748 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS261p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS261p-13CINOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 45.0 degrees Acq. time 1.311 sec Width 25000.0 Hz 100 repetitionsOBSERVE C13, 100.5671777 MHzDECOUPLE H1, 399.9500118 MHz Power 48 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 3 min, 51 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS268p-3
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS268p-3INOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 12 repetitionsOBSERVE H1, 399.9486780 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 49 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS211p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS211pc13INOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 45.0 degrees Acq. time 1.311 sec Width 25000.0 Hz 124 repetitionsOBSERVE C13, 100.5671799 MHzDECOUPLE H1, 399.9500118 MHz Power 48 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 4 min, 47 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS271p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS271p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 12 repetitionsOBSERVE H1, 399.9486778 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 49 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS271p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS271p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 1.311 sec Width 25000.0 Hz 80 repetitionsOBSERVE C13, 100.5671830 MHzDECOUPLE H1, 399.9500118 MHz Power 48 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 8 min, 25 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-245p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-245p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 60.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 499.4298997 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-106p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-106p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 53.3 degrees Acq. time 1.024 sec Width 32000.0 Hz 254 repetitionsOBSERVE C13, 125.5817502 MHzDECOUPLE H1, 499.4315638 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 40 min, 13 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-macrolide5
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-macrolide5INOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 500.0677748 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-175p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-175pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 500.0677750 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-macrolide5-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-macrolide5-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 60.0 degrees Acq. time 1.024 sec Width 32000.0 Hz 909 repetitionsOBSERVE C13, 125.5817483 MHzDECOUPLE H1, 499.4315638 MHz Power 46 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 5 hr, 1 min, 38 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
STANDARD PROTON PARAMETERS
Pulse Sequence: cyclenoe7.497
7.514
7.258
7.260
5.781
5.790
5.803
5.811
6.019
6.025
5.768
5.755
5.747
5.228
5.193
3.682
3.701
3.797
3.799
2.171
2.173
1.803
1.819
1.786
1.570
1.474
ppm234567
© 2009 Macmillan Publishers Limited. All rights reserved.
=====================================================================Injection Date : 4/27/2009 10:17:46 PM Seq. Line : 1Sample Name : EMS-III-158p Location : Vial 11Acq. Operator : sean Inj : 1Acq. Instrument : White Group HPLC Inj Volume : 1 µlDifferent Inj Volume from Sequence ! Actual Inj Volume : 2 µlAcq. Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 10:05:54 PM by seanAnalysis Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 9:44:31 PM by sean (modified after loading)Zorbax SB-CN 35C 40:60 H2O:MeCN2ml/min
min2 2.25 2.5 2.75 3 3.25 3.5 3.75 4
mAU
0
25
50
75
100
125
150
175
DAD1 C, Sig=214,4 Ref=off (DIAGNOSE\011-0101.D)
Are
a: 4
5.45
63
3.2
71
Are
a: 1
904.
45
3.6
73
===================================================================== Area Percent Report =====================================================================
Sorted By : SignalMultiplier : 1.0000Dilution : 1.0000Use Multiplier & Dilution Factor with ISTDs
Signal 1: DAD1 C, Sig=214,4 Ref=off
Peak RetTime Type Width Area Height Area # [min] [min] [mAU*s] [mAU] %----|-------|----|-------|----------|----------|--------| 1 3.271 MF 0.1698 45.45632 4.46177 2.3312 2 3.673 FM 0.1528 1904.45081 207.74139 97.6688
Totals : 1949.90712 212.20317
Results obtained with standard integrator!
Data File C:\HPCHEM\1\DATA\DIAGNOSE\011-0101.D Sample Name: EMS-III-158p
White Group HPLC 4/27/2009 9:44:38 PM sean Page 1 of 2
© 2009 Macmillan Publishers Limited. All rights reserved.
=====================================================================Injection Date : 4/27/2009 9:23:48 PM Seq. Line : 1Sample Name : EMS-III-115p Location : Vial 31Acq. Operator : sean Inj : 1Acq. Instrument : White Group HPLC Inj Volume : 1 µlDifferent Inj Volume from Sequence ! Actual Inj Volume : 2 µlAcq. Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 10:05:54 PM by seanAnalysis Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 9:47:29 PM by sean (modified after loading)Zorbax SB-CN 35C 40:60 H2O:MeCN2ml/min
min2 2.2 2.4 2.6 2.8 3 3.2 3.4 3.6 3.8
mAU
0
100
200
300
400
500
DAD1 C, Sig=214,4 Ref=off (DIAGNOSE\031-0101.D)
3.2
72
===================================================================== Area Percent Report =====================================================================
Sorted By : SignalMultiplier : 1.0000Dilution : 1.0000Use Multiplier & Dilution Factor with ISTDs
Signal 1: DAD1 C, Sig=214,4 Ref=off
Peak RetTime Type Width Area Height Area # [min] [min] [mAU*s] [mAU] %----|-------|----|-------|----------|----------|--------| 1 3.272 BV 0.1195 4779.23291 595.83240 100.0000
Totals : 4779.23291 595.83240
Results obtained with standard integrator!=====================================================================
Data File C:\HPCHEM\1\DATA\DIAGNOSE\031-0101.D Sample Name: EMS-III-115p
White Group HPLC 4/27/2009 9:47:32 PM sean Page 1 of 1
© 2009 Macmillan Publishers Limited. All rights reserved.
=====================================================================Injection Date : 4/27/2009 9:30:21 PM Seq. Line : 1Sample Name : EMS-III-136p Location : Vial 21Acq. Operator : sean Inj : 1Acq. Instrument : White Group HPLC Inj Volume : 1 µlDifferent Inj Volume from Sequence ! Actual Inj Volume : 2 µlAcq. Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 10:05:54 PM by seanAnalysis Method : C:\HPCHEM\1\METHODS\COLUMNS\REVERSE\ACHIRAL\C8\EMS40H2O.MLast changed : 4/27/2009 9:35:19 PM by sean (modified after loading)Zorbax SB-CN 35C 40:60 H2O:MeCN2ml/min
min2 2.2 2.4 2.6 2.8 3 3.2 3.4 3.6 3.8
mAU
0
20
40
60
80
100
DAD1 C, Sig=214,4 Ref=off (DIAGNOSE\021-0101.D)
3.2
74
3.6
76
===================================================================== Area Percent Report =====================================================================
Sorted By : SignalMultiplier : 1.0000Dilution : 1.0000Use Multiplier & Dilution Factor with ISTDs
Signal 1: DAD1 C, Sig=214,4 Ref=off
Peak RetTime Type Width Area Height Area # [min] [min] [mAU*s] [mAU] %----|-------|----|-------|----------|----------|--------| 1 3.274 BV 0.1211 912.75916 112.89211 41.9133 2 3.676 VV 0.1460 1264.97192 126.26372 58.0867
Totals : 2177.73108 239.15583
Results obtained with standard integrator!
Data File C:\HPCHEM\1\DATA\DIAGNOSE\021-0101.D Sample Name: EMS-III-136p
White Group HPLC 4/27/2009 9:40:02 PM sean Page 1 of 2
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-63p-5-dia-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-III-63p-5-dia-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 500.0677750 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-83p-dia-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-III-83p-dia-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 65.9 degrees Acq. time 1.086 sec Width 30165.9 Hz 1064 repetitionsOBSERVE C13, 125.6472855 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 5 hr, 4 min, 51 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
STANDARD PROTON PARAMETERS
Pulse Sequence: cyclenoe7.260
5.946
5.730
5.521
5.204
5.169
2.151
1.568
1.561
1.501
1.255
0.967
0.952
ppm1234567
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
F1 (ppm)
102030405060708090
F2(ppm)1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
© 2009 Macmillan Publishers Limited. All rights reserved.
F1 (ppm)
110111112113114115116117118119120121122
F2(ppm)
4.5
5.0
5.5
6.0
6.5
7.0
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-233p-a
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureOperator: user1dFile: EMS-II-233p-aINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 64.3 degrees Acq. time 4.665 sec Width 7024.9 Hz 4 repetitionsOBSERVE H1, 499.6906564 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 38 sec
ppm-1-01234567891011
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-233p-a-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureOperator: user1dFile: EMS-II-233p-a-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 61.0 degrees Acq. time 1.086 sec Width 30165.9 Hz 184 repetitionsOBSERVE C13, 125.6473166 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 30 min, 34 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-233p-b
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-233p-bINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 500.0677748 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-233p-b-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureOperator: user1dFile: EMS-II-233p-b-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 61.0 degrees Acq. time 1.086 sec Width 30165.9 Hz 198 repetitionsOBSERVE C13, 125.6473166 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 30 min, 34 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-173p-2
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-173p-2INOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 59.9 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 399.9486778 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-202468101214
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-111p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-III-111p-13CINOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 65.9 degrees Acq. time 1.086 sec Width 30165.9 Hz 1983 repetitionsOBSERVE C13, 125.6473166 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 5 hr, 49 min, 13 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-108p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-III-108p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 499.4298995 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-108p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-III-108p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 65.9 degrees Acq. time 1.086 sec Width 30165.9 Hz 541 repetitionsOBSERVE C13, 125.6472855 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 16 hr, 55 min, 57 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-109p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-109p-pubINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 46.8 degrees Acq. time 4.665 sec Width 7024.9 Hz 20 repetitionsOBSERVE H1, 499.6964458 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 3 min, 13 sec
ppm-1-01234567891011
© 2009 Macmillan Publishers Limited. All rights reserved.
13C OBSERVE
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-109p-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 45.0 degrees Acq. time 1.311 sec Width 25000.0 Hz 235 repetitionsOBSERVE C13, 100.5671754 MHzDECOUPLE H1, 399.9500118 MHz Power 48 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 10 hr, 31 min, 57 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-243p-2-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-243p-2-pubINOVA-500 "sunds1"
Relax. delay 10.000 sec Pulse 60.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 14 repetitionsOBSERVE H1, 499.4298997 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 3 min, 17 sec
ppm-2024681012
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-243p-2-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-243p-2-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 60.0 degrees Acq. time 1.024 sec Width 32000.0 Hz 1561 repetitionsOBSERVE C13, 125.5817473 MHzDECOUPLE H1, 499.4315638 MHz Power 46 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 5 hr, 1 min, 38 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-257p-2
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-II-257p-2INOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 8 repetitionsOBSERVE H1, 500.0677748 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 1 min, 12 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-II-257p-2-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-II-257p-2-13CINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 60.0 degrees Acq. time 1.024 sec Width 32000.0 Hz 1085 repetitionsOBSERVE C13, 125.5817483 MHzDECOUPLE H1, 499.4315638 MHz Power 46 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 5 hr, 1 min, 38 sec
ppm020406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-85p-pub
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-III-85p-pubINOVA-500 "sunds1"
Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz Single scanOBSERVE H1, 500.0677750 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 4 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-85p-13C
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureUser: 1-14-87File: EMS-III-85p-13CINOVA-500 "sunds1"
Relax. delay 1.000 sec Pulse 65.9 degrees Acq. time 1.086 sec Width 30165.9 Hz 1458 repetitionsOBSERVE C13, 125.6473166 MHzDECOUPLE H1, 499.6923275 MHz Power 44 dB continuously on WALTZ-16 modulatedDATA PROCESSING Line broadening 1.0 HzFT size 65536Total time 2 hr, 54 min, 37 sec
ppm20406080100120140160180200220
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-91p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-III-91pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 61.6 degrees Acq. time 4.665 sec Width 7024.9 Hz 4 repetitionsOBSERVE H1, 499.6906570 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 38 sec
ppm-1-01234567891011
© 2009 Macmillan Publishers Limited. All rights reserved.
EMS-III-92p
Pulse Sequence: s2pul
Solvent: CDCl3 Ambient temperatureFile: EMS-III-92pINOVA-500 "sunds1"
Relax. delay 5.000 sec Pulse 90.0 degrees Acq. time 4.096 sec Width 8000.0 Hz 4 repetitionsOBSERVE H1, 500.0677750 MHzDATA PROCESSING Line broadening 0.3 HzFT size 65536Total time 0 min, 36 sec
ppm-2-10123456789101112
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
© 2009 Macmillan Publishers Limited. All rights reserved.
