Supplementary Material. Chemical ligation from O-acyl isopeptides via 8- and 11-membered cyclic transition states
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1 Supplementary Material Chemical ligation from -acyl isopeptides via 8- and 11-membered cyclic transition states Siva S. Panda, a Mohamed Elagawany, a,b Hadi M. Marwani, c Eray Çalışkan, a Mirna El Khatib, a Alexander liferenko, a Khalid A. Alamry, c and Alan R. Katritzky* a,c a Center for Heterocyclic Compounds, Department of Chemistry, University of Florida, Gainesville, FL (USA) b Department of rganic Chemistry, College of Pharmacy, Misr University for Science and Technology, Al-Motamayez District, P.. Box: 77, Egypt c Department of Chemistry, King Abdulaziz University, Jeddah, 21589, Saudi Arabia katritzky@chem.ufl.edu Table of Contents 1. 1 H NMR and 13 C NMR spectra for compounds S2 2. HPLC chromatograms and MS Spectra for 5a and 6a S42 3. HPLC chromatograms and MS Spectra for 5f and 6f S 4. HPLC chromatograms and MS Spectra for 5c and 6c S62 5. HPLC chromatograms and MS Spectra for 9a and a S64 Page S1
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42 HPLC chromatograms and MS Spectra for 5a and 6a Page S42
43 Figure S1. Lig8 NonAq, MW 9-A E:\-Spec\-Data\Seq /13/11 3:41:29 PM Lig8NNAQ, mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms SEQ # RT: AV: 4 SB: NL: 1.11E7 T: - c ESI sid=1. Full ms [ 1.-.] SEQ # RT: AV: 5 SB: NL: 9.1E5 F: - c ESI sid=3. Full ms [ 6.-.] Page S43
44 Figure S2. MW 9-B, Lig8 NonAq E:\-Spec\-Data\Seq /13/11 3:41:29 PM Lig8NNAQ, mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms SEQ #23-61 RT: AV: 5 SB: NL: 1.62E7 T: - c ESI sid=1. Full ms [ 1.-.] SEQ #28-53 RT: AV: 3 SB: NL: 8.26E5 F: - c ESI sid=3. Full ms [ 6.-.] Page S44
45 Figure S3. Lig8 NonAq: HPLC/UV/(-)ESI-MS and MSn chromatograms for the MW 9 compounds E:\-Spec\-Data\Seq /13/11 3:41:29 PM Lig8NNAQ, mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms RT: Relative Intensity Tim e (m in) Page S NL: 3.19E7 Base Peak F: - c ESI sid=1. Full ms [ 1.-.] MS SEQ NL: 1.68E6 Base Peak F: - c ESI sid=3. Full ms [ 6.-.] MS SEQ NL: 3.19E7 = F: - c ESI sid=1. Full ms [ 1.-.] MS SEQ NL: 1.67E7 Base Peak F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] MS SEQ NL: 1.99E6 Base Peak F: - c sid=2. d Full ms3 8. MS SEQ NL: 1.17E-1 UV Analog SEQ
46 Figure S4. MW 9 compounds: (-)ESI-MS/MS (top and 3rd) and MS/MS/MS (2nd and bottom) for the MW 9-A (RT min) and MW 9-B (RT 23.7 min) E:\-Spec\-Data\Seq /13/11 3:41:29 PM Lig8NNAQ, mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms SEQ # RT: AV: 3 NL: 2.86E6 F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] SEQ # RT: AV: 3 NL: 6.14E5 T: - c sid=2. d Full ms3 8.@ @37. [ ] SEQ # RT: AV: 4 NL: 1.2 1E 7 F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] SEQ # RT: AV: 3 NL: 1.57E6 T: - c sid=2. d Full ms3 8.@ @37. [.-675.] Page S46
47 Figure S5. Lig8 NonAq: MW 9 isomers. The two MW 9 isomers were well separated and were characterized relatively uniquely by their (-)ESI-MS/MS product ions as shown below. The MW 9-A was the starting material while MW 9-B was SEQ /13/11 3:41:29 PM Lig8NNAQ, mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms RT: NL: 3.19E7 = F: - c ESI sid=1. Full ms [ 1.-.] MS SEQ (-)ESI-MS, (-)ESI-MS/MS 8 => 174 RT: BP: MW 9-A NL: 3.34E6 = F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] MS SEQ (-)ESI-MS/MS 8 => 334 RT: BP: MW 9-B NL: 1.69E7 = F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] MS SEQ Time (min) product. Scheme 1 shows the likely formation of the two product ions below Page S47
48 Scheme S1. The two MW 9 compounds are characterized by the formation of different major products ions from the (-)ESI- MS/MS collision-induced dissociation (CID) of their 8 [M-H]- ions. 1. Molecular Formula = C 19 H 27 N 3 7 Monoisotopic Mass = Da H 2 N H HN NH H 3 C CH 3 CH 3 (-)ESI 8 [M-H]- CID - H 3 C NH 174 CH 3 CH 3 solution phase chemistry H 3 C H 3 C CH 3 NH N HN (-)ESI 8 [M-H]- CID HN HN HN H H - H Molecular Formula = C 19 H 27 N 3 7 Monoisotopic Mass = Da 334 Page S48
49 Figure S6. Lig8 SM, MW 9, RT 19. min: With (-)ESI-MS, the MW 9 produced an 8 [M-H]- ion (top) which was dissociated to 174 (middle) which was further dissociated to (bottom). The RT and MSn spectra match those of the MW 9-A compound of Lig8 NonAq SEQ /13/11 6:41:18 PM Lig8 SM; mg/ml; 5 ul injected Hydro-RP;.2;:()>55:45(15)>25:75(45)>5:95(-)/254 nm/(-)esi-ms SEQ #812-6 RT: AV: 13 NL: 2.1E7 T: - c ESI sid=1. Full ms [ 1.-.] SEQ # RT: AV: NL: 5.95E6 F: - c ESI sid=2. Full ms2 8.@37. [ 1.-4.] SEQ # RT: AV: NL: 1.13E6 T: - c sid=2. d Full ms3 8.@ @37. [ ] Page S49
50 HPLC chromatograms and MS Spectra for 5f and 6f. Figure S7. MW 423, Rt 38.4 min: This was the most abundant MS and UV peaks. SEQ /22/11 7:31:19 AM ME36 in ul MeH; 5 ul injected XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi RT: NL: 1.22E Base Peak F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 2.25E RT: MA: BP: RT: MA: BP: 446. RT: MA: BP: MW Base Peak F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ NL: 1.22E8 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 2.65E7 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 7.15E7 = F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ NL: 8.93E-2 Intensity UV Analog SEQ Time (min) Page S
51 Figure S8.Sample ME36, MW 423. Due to the high concentration, self-adduct ions ( 8-958; 13-14) were also formed in addition to the 424 [M+H]+ and 445 [M+Na]+. Note the presence of other compounds also, e.g SEQ /22/11 7:31:19 AM ME36 in ul MeH; 5 ul injected XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 6 NL: 5.63E7 T: + c ESI sid=1. Full ms [ ] SEQ # RT: AV: 5 NL: 1.45E7 F: + c ESI sid=3. Full ms [ 7.-.] Page S51
52 Figure S9.Sample ME36, MW 423. (+)ESI-MSn. SEQ /22/11 7:31:19 AM ME36 in ul MeH; 5 ul injected XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 6 NL: 5.63E7 T: + c ESI sid=1. Full ms [ ] SEQ # RT: AV: 3 NL: 5.2E7 F: + c ESI sid=2. Full ms2 424.@37. [ ] SEQ # RT: AV: 2 NL: 2.E7 T: + c sid=2. d Full ms3 424.@ @37. [.-745.] Page S52
53 Figure S. ME37, MW 423 compounds: (+)ESI mass spectra of RT 38.6 min (top) and RT 39.5 min (bottom) The 324 and 368 are fragment ions. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 2 SB: , NL: 2.12E8 T: + c ESI sid=1. Full ms [ ] SEQ #1551 RT: 39. AV: 1 SB: , NL: 2.49E7 T: + c ESI sid=1. Full ms [ ] Page S53
54 Figure S11. ME37, MW 423 compounds: (+)ESI mass spectra ( 7-) of RT 38.6 min (top) and RT 39.5 min (bottom).. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 3 SB: , NL: 7.87E6 F: + c ESI sid=3. Full ms [ 7.-.] SEQ # RT: AV: 2 SB: , NL: 9.6E6 F: + c ESI sid=3. Full ms [ 7.-.] Page S54
55 Figure S12. MW 423 RT 38.5 min: (+)ESI-MS/MS of the 424 [M+H]+ ions from ME37 (top) and ME 36 (bottom) were identical. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 3 NL: 1.19E8 F: + c ESI sid=2. Full ms2 424.@37. [ ] 368. ME SEQ # RT: AV: 2 NL: 6.55E7 F: + c ESI sid=2. Full ms2 424.@37. [ ] 368. ME Page S55
56 Figure S13. MW 423 compounds in ME37. (+)ESI-MS/MS (top and 3 rd ) and MS/MS/MS (2 nd and 4 th ) for the 38.6 min (top 2) and RT 39.5 min (bottom 2) MW 423 compounds. The corresponding spectra are near identical. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 2 NL: 1.4 1E8 F: + c ESI sid=2. Full ms2 424.@37. [ ] m/ z SEQ # RT: AV: 2 NL: 5.38E7 T: + c sid=2. d Full ms3 424.@ @37. [.-745.] m/ z SEQ # RT: AV: 2 NL: 1.36E7 F: + c ESI sid=2. Full ms2 424.@37. [ ] m/ z SEQ # RT: AV: 2 NL: 5.34E6 T: + c sid=2. d Full ms3 424.@ @37. [.-745.] m/ z Page S56
57 Figure S14. MW 423 compounds, integrated peak areas. The corresponding areas should be summed. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi RT: RT: MA: BP: 368. RT: 39. MA: BP: 368. NL: 2.15E8 = F: + c ESI sid=1. Full ms [ ] MS SEQ RT: MA: BP: RT: 39. MA: BP: 424. NL: 2.E8 = F: + c ESI sid=1. Full ms [ ] MS SEQ RT: MA: BP: RT: MA: BP: NL: 5.47E7 = F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ NL: 2.1E8 = F: + c ESI sid=2. Full ms2 424.@37. [ ] MS SEQ Time (min) Page S57
58 Figure S15. MW 176: This compound was not retained on the HPLC column and eluted at RT 2.8 min. Due to its ion-chemistry and abundance, it produced mostly self-adduct ions. Note also that it produced 221 [M-H+Na+Na]+ and the neutral for adduction was the MW 198 [M-H+Na]. There also appeared to be CH2 homolog at 235. The adduct ions were likely homo (all MW 198 or all MW 212) and hetero(mixture of the 2 ions). SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ #3-116 RT: AV: 2 NL: 2.39E6 T: + c ESI sid=1. Full ms [ ] SEQ # RT: AV: 2 SB: , NL: 1.32E6 F: + c ESI sid=3. Full ms [ 7.-.] RT: Time (min) Page S58 NL: 8.52E3 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 5.38E5 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 3.E6 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 6.85E6 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 2.46E7 TIC F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ NL: 2.65E4 Base Peak F: + c ESI sid=4. Full ms2 177.@37. [.-.] MS SEQ
59 Figure S16. MW 176: (+)ESI-MS (top) and MS/MS f 177 (very weak; middle) and of 419 [2(M-H+Na)+Na]+ (bottom). SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ #3-116 RT: AV: 2 NL: 2.39E6 T: + c ESI sid=1. Full ms [ ] SEQ #1 RT: 2.76 AV: 1 SB: , NL: 2.6E3 F: + c ESI sid=4. Full ms2 177.@37. [.-.] SEQ #5 RT: 2. AV: 1 NL: 1.14E6 T: + c sid=1. d Full ms @37. [ 5.-8.] Page S59
60 Figure S17. MW 176: HPLC/(+)ESI-MS ion-peaks integrated. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi RT: RT: 2.79 MA: BP: RT: 2.79 MA: BP: RT: 2.97 MA: 8674 BP: RT: 2.78 MA: BP: 815. RT: 2.78 MA: 7487 BP: 13.1 NL: 5.45E6 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 3.E6 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 3.7E6 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 5.42E6 = F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ NL: 4.29E6 = F: + c ESI sid=3. Full ms [ 7.-.] MS SEQ Time (min) Page S
61 Figure S18. MW 6? The MW 6 should have produced an 671 [M+H]+ and 693 [M+Na]+ ions. There were no correlating ion-peaks for these two ions. There was a very small 671 ion-peak at RT but the signal was too low to be conclusive. The (+)ESI mass spectra for the relataively abundant 693 ion-peak at Rt does not indicate an 671. The presence of an 715 suggests this is a MW 692 compound. I have integrated the 693 ion-peak. SEQ /22/11 5:54:32 AM ME37; 5 ul XTerra MS C18;.15;:()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 2 SB: , NL: 4.49E7 T: + c ESI sid=1. Full ms [ ] RT: NL: 4.E5 = F: + c ESI sid=1. Full ms [ ] MS SEQ RT: MA: BP: NL: 2.57E7 = F: + c ESI sid=1. Full ms [ ] MS SEQ Time (min) Page S61
62 HPLC chromatograms and MS Spectra for 5c and 6c Figure S19. MW 333, RT 18.1 min. The MW 333 compound formed 334 [M+H]+, 356 [M+Na]+ and 378 [M- H+2Na]+ ions (top) with the latter being indicative of an acidic proton. The 334 was readily dissociated to 278 (middle) which was dissociated further to 234, and several other secondary product ions (bottom). SEQ //11 1:27:36 PM ME33 in ul MeH; 5 ul injected Hydro-RP;.2;95:5()>5:95(45-)/254 nm/(+)esi SEQ # RT: AV: 5 SB: NL: 1.54E7 F: + c ESI sid=1. Full ms [ ] SEQ # RT: AV: 8 NL: 2.53E7 F: + c ESI Full ms2 334.@37. [.-3.] SEQ # RT: AV: 5 NL: 6.69E6 T: + c d Full ms3 334.@ @37. [ ] Page S62
63 Figure S. MW 333 compounds. A new MW 333 compound eluted at RT.32 min (shaded peak). The unshaded 334 and 334 => 279 peaks are due to SM compounds SEQ //11 11:47:23 AM ME34 in ul MeH; 5 ul injected Hydro-RP;.2;95:5()>5:95(45-)/254 nm/(+)esi RT: RT:.32 BP: RT:.27 BP: NL: 3.E7 Base Peak F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 1.72E7 = F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 4.65E7 = F: + c ESI Full ms2 334.@37. [.-3.] MS SEQ NL: 1.19E-1 UV Analog SEQ Intensity Time (min) Page S63
64 HPLC chromatograms and MS Spectra for 9a and a Scheme S2. taken from the submitted reaction NH 2 HN LIG11SM (SEQ-16928) Molecular Formula = C 21 H N 4 8 Monoisotopic Mass = u H HN NH H 3 C CH 3 CH 3 Products: SEQ LIG11NN-AQ SEQ-169 LIG11AQ7.65 NH CH 3 NH CH 3 NH 2 HN H 3 C CH 3 HN H 3 C CH 3 HN HN HN HN H HN H H HN NH H 3 C CH 3 CH 3 H HN H Molecular Formula = C 21 H N 4 8 Monoisotopic Mass = Da Molecular Formula = C 28 H 41 N 5 11 Monoisotopic Mass = Da Molecular Formula = C 16 H 22 N 4 6 Monoisotopic Mass = Da Page S64
65 Figure S21. LIG11SM, MW 466, RT min. The MW 466 produced 467 [M+H]+, 489 [M+Na]+ and 511 [(M- H+Na)+Na]+ ions (top). The latter is characteristic of compounds with acidic protons, e.g. RCH SEQ /1/11 6:54:43 AM LIG11SM in ul ACN; ul injected Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(+)esi-ms SEQ #966-1 RT: AV: 4 SB : , NL: 9.46E6 T: + c ESI sid=2. Full ms [ 2.-.] SEQ # 964 RT: 25.3 AV: 1 NL: 5.72E6 T: + c sid=2. d Full ms @37. [ 1.-9.] SEQ # 965 RT: 25.6 AV: 1 NL: 1.32E6 T: + c sid=2. d Full ms @ @37. [ ] Page S65
66 Figure S22. LIG11NNAQ, MW 466, RT min. The MW 466 product was expected to produce 467 [M+H]+ and 489 [M+Na]+ ions. The mass chromatograms show only one potential MW 466 compound at RT SEQ /1/11 :8:28 AM LIG11NNAQ; ul Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(+)esi-ms RT: Intensity RT: BP: 467. RT: BP: Time (min) NL: 4.17E7 Base Peak F: + c ESI sid=1. Full ms [ ] MS SEQ NL: 3.13E7 Base Peak F: + c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 4.33E5 = F: + c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 6.47E6 = F: + c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 4.69E-1 UV Analog SEQ Page S66
67 Figure S23. LIG11 NNAQ via HPLC/UV/(-)ESI-MSn, MW 466, RT min. The tentative MW 466 detected via (+)ESI-MS above produced predominantly an 465 [M-H]- ion under (-)ESI-MS conditions and thus confirmed it as being a MW 466 compound SEQ /1/11 11:43:24 AM LIG11NNAQ; ul Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms SEQ # RT: AV: 7 SB: , NL: 1.13E7 T: - c ESI sid=2. Full ms [ 3.-.] RT: RT: BP: NL: 1.12E7 Base Peak F: - c ESI sid=1. Full ms [ ] MS SEQ NL: 1.94E7 Base Peak F: - c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 1.94E7 = F: - c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 5.29E-1 UV Analog SEQ Intensity Time (min) Page S67
68 Figure S24. HPLC/(-)ESI-MS mass chromatograms of 465. MW 466 compounds in (top to bottom): LIG11SM, LIG11NNAQ and LIG11 AQ nly a very minor amount of MW 466 was detected in the LIG11 AQ7.65 sample. Note the products eluted prior to the starting material. SEQ /1/11 4:14:2 PM LIG11SM in ul ACN; ul injected Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms RT: RT: BP: LIG11SM, MW RT: BP: LIG11NNAQ, MW 466 NL: 3.E6 = F: - c ESI sid=2. Full ms [ 3.-.] MS SEQ NL: 1.94E7 = F: - c ESI sid=2. Full ms [ 3.-.] MS SEQ RT: BP: LIG11 AQ 7.65, MW Time (min) NL: 1.63E5 = F: - c ESI sid=2. Full ms [ 3.-.] 38.5 MS SEQ Page S68
69 Figure S25. (-)ESI-MS/MS of the 465 [M-H]- ions of the MW 466 compounds in (top to bottom): LIG11SM, LIG11NNAQ and LIG11 AQ While it was expected that the starting material and products were different, the two MW 466 products also produced different dissociation ions. SEQ /1/11 4:14:2 PM LIG11SM in ul ACN; ul injected Hypurity 2. C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms SEQ # RT: AV: 8 NL: 6.88E4 F: - c ESI sid=2. Full ms2 465.@37. [ ] SEQ # RT: AV: 5 NL: 1.54E7 F: - c ESI sid=2. Full ms2 465.@37. [ ] SEQ # RT: AV: 3 SB : NL: 1.29E5 F: - c ESI sid=2. Full ms2 465.@37. [ ] Page S69
70 Figure S26. LIG11SM, MW 466, (-)ESI-MSn of the 465 [M-H]- ion. 3. SEQ /1/11 4:14:2 PM LIG11SM in ul ACN; ul injected Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms SEQ # RT: AV: 8 NL: 6.88E4 F: - c ESI sid=2. Full ms2 465.@37. [ ] SEQ # 959 RT: AV: 1 NL: 3.58E4 T: - c sid=2. d Full ms3 465.@ @37. [ 5.-8.] SEQ # RT: AV: 3 NL: 1.14E5 T: - c sid=2. d Full ms3 465.@ @37. [ ] Page S
71 Figure S27. LIG11 NN-AQ, MW 466, RT min: (-)ESI-MS/MS (top) and MS/MS/MS (bottom) of the 465 [M-H]- ion. 4. SEQ /1/11 11:43:24 AM LIG11NNAQ; ul Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms SEQ # RT: AV: 5 NL: 1.54E7 F: - c ESI sid=2. Full ms2 465.@37. [ ] SEQ # RT: AV: 5 NL: 3.24E6 T: - c sid=2. d Full ms3 465.@ @37. [ ] Page S71
72 Figure S28. LIG11 AQ7.65, MW 466, RT min. The 465 [M-H]- was very minor in its (-)ESI-MS (top). The dominant ion was 5. It is not uncommon to see [M+59]- ions where 59 is the acetate anion (from acetic acid often used in the mobile phase). Might the 465 be an [M+59]- ion of a MW 6 compound? The 465 was dissociated to 433, 397 and 365 ( 397 may be background). The 433 was dissociated further to 365 and 246 (bottom). SEQ /1/11 2:41:12 PM LIG11AQ7.65, ul Hypurity C8;.2;:()>:(15)>:(45-)/254 nm/(-)esi-ms SEQ # RT: AV: 3 SB: , NL: 2.32E6 T: - c ESI sid=2. Full ms [ 3.-.] SEQ # RT: AV: 2 SB: , NL: 1.4 3E5 F: - c ESI sid=2. Full ms2 465.@37. [ ] SEQ # 869 RT: AV: 1 NL: 5.83E4 T: - c sid=2. d Full ms3 465.@ @37. [ ] Page S72
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