th  - 1988 - 51st ENC Conference

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21 DETECTION OF LONG-RANGE IH-19F COUPLINGS USING A HETERONUCLEAR [ EQUIVALENT OF THE COSY PULSE SEQUENCE. Donald W.Hughes and Alex D.Bain, Department of Chemistry, McMaster University, Hamilton, Ontario. Canada. LSS 4MI. Heteronuclear chemical shift correlation has become an indispensable technique for assigning the spectra of natural products. The original pulse sequence (I) IH : D1 - 90 ° - t I - 90 ° X : 90 ° - ACQ has been largely neglected by spectroscopists because of the complications arising from heteronuclear coupling in both dimensions. Recently this pulse sequence was reexamined with a phase-sensitive modification (2). The principle advantage this heteronuclear correlation (HETCOSY) method is that like the homonuclear COSY experiment it is a robust technique i.e.resistant to errors. HETCOSY can produce correlations between protons and X nuclei without prior knowledge of X-IH coupling constants. This feature makes HETCOSY useful for establishing correlations between protons and X nuclei such as 19F and 31p, especially in cases where the X-IH couplings are not well resolved. The present study deals with the application of HETCOSY in identifying which fluorine nuclei are responsible for long-range IH-19F couplings in corticosteriods related to fluocinonide. I. A.A.Maudsley and R.R. Ernst. Chem. Phys. Lett.50, 368 (1977) 2. A.D. Bain. J. Magn. Reson. In press (1988) I -- 22 I STUDIES OF PHOSPHORYLATED SITES IN PROTEINS USING IH - David H. Live and Dale E. Edmondson # 31p 2-DIMENSIONAL NMR *Department of Chemistry and #Department of Biochemistry, Emory University, Atlanta, GA 30322 The application of proton detected IH - 31p multiquantum 2-dimensional NMR to directly studying the phophorylated sites of proteins is demonstrated here. This approach works well for proteins up to molecular weight of about 40 kD in spite of the fact ~at the 2D spectrum is mediated by small 3 or more bond couplings between ~P and protons on phosphorylated amino acid residues. Results are presented for the protein Azotobacter flavodoxin, an electron carrier in nitrogen fixation. The results provide the first direct evidence for the existence of a phosphate diester linkage between a seryl and a threonyl residue in the protein. Data from this protein are compared to that from phosphoserine, phosphothreonine and ovalbumin. 108
2 3- I A SOLID-STATE 2H and 13C NMR STUDY OF THE STRUCTURE OF POLYANILINES: Samuel Kaplan* and Esther M. Conwell, Xerox Webster Research Center, 800 Phillips Rd. 011ll-39D, Webster, NY lt1580; Alan F. Richter and Alan G. MacDiarmid" Department of Chemistry, University of Permsylania" Philadelphia, PA 1910tl. Polyaniline, synthesized by the electrochemical or chemical oxidative polymerization of aniline, can exist as a number of unique structures of the form . . . . . ly~ . . . . . . x 1A 2A where 0-
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29 th �� - 1988 Rochester
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PROGRAM: This conference program ha
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The Executive Committee of the 29th
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A A 0 0 ,-..1 I Z Z 0 "c N "1" i 0
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Restaurants in Rochester Restaurant
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8:30 a.m. 8:35- 10:05 10:05 - 10:25
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8:30 a.m. 8:35 a.m. 9:05 a.m. 9:15
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f~ I UNTRUNCATIO~I OF DIPOLE-DIPOLE
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MON 9:25 HIGH RESOLUTION ELECTROPHO
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• . r, 10:25 a.m. 10:55 a.m. 11:0
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~'-O-i 0 N i0:55 MEASUREMENTS OF TW
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MON 11:3S 12D CHEMICAL SHIFT ANISOT
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7:30 p.m. 8:00 p.m. 8:10 p.m. 8:40
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HON Eve 8:00 The 13C Relaxation Beh
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THE WORLD AND WONDERS OF 3H NMR SPE
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8:30 a.m. 9:00 a.m. 9:10 a.m. 9:20
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TWO DIMENSIONAL LINEAR PREDICTION N
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TUE 9"20 ] 2D ROTATING FRAME SPECTR
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10:40 a.m. 11:00 a.m. 11:20 a.m. 11
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TUE ii'00 J WATER SUPPRESSION TECHN
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TUE 11:30 J FREQUENCY SWITCHED INVE
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7:30 p.m. 8:00 p.m. 8:30 p.m. 8:50
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• . r T[-~-UE ~ t~ve 8:00! 63,65C
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TUE Eve 8-50 } Cu NQR OF YBa2Cu30 x
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~X [I'IED 8:30 I REMOVAL OF EXTRANE
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. r WED 9:25 ] A STATIC NMR IMAGE O
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WED 9" 45 IFLUID AND SOLID STATE NM
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i MULTIVOLUME SELECTIVE SPECTROSCOP
Page 57 and 58: [WED 11-10 I SELF SHIELDED GRADIENT
Page 59 and 60: [WED 11:45 ] ANGIOGRAPHY USING MAGN
Page 61 and 62: THU 8:30 "TETHERED" BIOLOGICAL SYST
Page 63 and 64: • / I DYNAMICS OF THE GRAMICIDIN
Page 65 and 66: I THU 9:40 I NMR STUDIES OF ANTI-SP
Page 67 and 68: THU 10"2S I NEW TECHNIQUES POR DYNA
Page 69 and 70: I THU 11 : 05 I DYNAMIC NUCLEAR POL
Page 71 and 72: THIS SECTION CONTAINS A LISTING OF
Page 73 and 74: 9 ELIMINATION OF PHASE ROLL, SOLVEN
Page 75 and 76: 25 NUCLEAR MAGNETIC RESONANCE STUDI
Page 77 and 78: ~k 41 A HYPO-RELAXATION AGENT; SIMU
Page 79 and 80: 57 STRUCTURAL STUDIES OF LIPIDS IN
Page 81 and 82: 73 THE AUTOMATED NMR LABORATORY; SP
Page 83 and 84: 89 13C NMR ASSIGNMENTS OF DNA OLIGO
Page 85 and 86: 105 EVALUATION OF DOUBLE TUNED CIRC
Page 87 and 88: 121 BROADBAND SPIN DECOUPLING IN TH
Page 89 and 90: 137 TWO-DIMENSIONAL 13C{15N}, 13C{1
Page 91 and 92: 153 NMR CHARACTERIZATION OF THE SOL
Page 93 and 94: 169 SPECTROSCOPY WITH EXACT APODIZA
Page 95 and 96: 185 PARSING THE EDITED 1H NMR SIGNA
Page 97 and 98: . z 201 THE CORRELATION OF 1H-19F C
Page 99 and 100: i m 3 I 31p SOLID STATE NMR STUDIES
Page 101 and 102: CALCULATION OF 2951MAS NMR CHEMICAL
Page 103 and 104: AN NMR STUDY OF MISCIBLE BLENDS IN
Page 105 and 106: 15 II9F CRAMPS OF INORGANIC FLUORID
Page 107: 19 I DIPOLARAND SPIN-ROTATION POLAR
Page 111 and 112: 27 1 COLLECTION OF PHOSPHORUS-31 NM
Page 113 and 114: 31 DELAYED REFOCUSSING TWO-DIMENSIO
Page 115 and 116: 35 DYNAMIC NUCLEAR POLARIZATION STU
Page 117 and 118: I 39 2D NMR STUDIES AT 600 MHZ OF A
Page 119 and 120: 43 Coherent Averaging Theory Under
Page 121 and 122: 46 CARBON-13 SPECTRAL ASSIGNMENTS O
Page 123 and 124: a b 48 SEMUT SPECTRAL EDITING, CALI
Page 125 and 126: '--- V 5 2 j INTERCONWERSION OF VAL
Page 127 and 128: [ ~ THE SOURCE OF AN ARTIFACT IN TH
Page 129 and 130: 60 GLUCOSE METABOLISM IN PERFUSED H
Page 131 and 132: . °- F 64 I MICROSCOPIC IMAGING OF
Page 133 and 134: 68 69 CONFORMATIONAL ANALYSIS via V
Page 135 and 136: 72 I SCUBA, A MAY TOHARDS COMPLETE
Page 137 and 138: 76 NMR CHARACTERIZATION OF THE GLYP
Page 139 and 140: 8o I HIGH RESOLUTION MR IMAGING AT
Page 141 and 142: A PROBE WITH HIGHER DECOUPLING EFFI
Page 143 and 144: 88 I SOLID STATE ll3cd I~CLEAR }~GE
Page 145 and 146: - - 92 l CHARACTERIZATION OF NORMAL
Page 147 and 148: 96 AN EVALUATION OF NEW PROCESSING
Page 149 and 150: . . I00 I NOVEL RESONATOR DESIGNS,
Page 151 and 152: 104 TAYLOR TRANSFORMATION OF 2D NMR
Page 153 and 154: 108 PERFORMANCE COMPARISON OF DOUBL
Page 155 and 156: RECENT EXTENSIONS OF NOESYSIM, A PR
Page 157 and 158: 116 ] NODIFICATIONS TO A JEOL GX270
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I 12 o I SPECIATION OF WATER IN GLA
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124 I A COMPLETELY INTEGRATED NETWO
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I-- 1 2 8 IVOLUME-SELECTIVE SIGNAL
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-- is 2 I NATURAL ABUNDANCE 13 C an
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. ° THREE-DIMENSIONAL STRUCTURE OF
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~-'-- 140 DIRECT OBSERVATION OF LON
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144 I I IH AND 13C REFOCUSED GRADIE
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~ (POSTER ABSTRACT) BARBARA LYONS/C
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1 52 I ~IR STUDY OF NAPHTHALENE TRA
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is6 I ROTATING FRAME COHERENCE TRAN
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16 0 I A 27AL MAS STUDY OF AMORPHOU
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164 I MODIFICATIOH OF A BRUKER WH-3
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IN VIVO 31p AND IH NMR SPECTROSCOPY
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. r 172 JMAGIC ANGLE SPINNING SEPAR
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2 . ° I- 176 I Michael A. Kennedy
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. o . o 180 l17o/Is NMR MICROSCOPY
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To be presented at the 29th Experim
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INHIBITION OF ALANINE RACEMASE BY T
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192 RESOLUTION ENHANCEMENT OF PHOSP
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196 1 TR FLUOROETHOXY DERIVATIVES:
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200 INTERPRETAT IION OF 13 C NHR MI
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204 RECENT PROGRESS IN HIGH RESOLUT
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Page No. ACEVEDO, H F 165 ACKERMAN,
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1:~ge No. GUO, D 200 GUO, W 196 GUO
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OPELLA, S J ORENDT, A M OTTING, G P
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ZLOTNIK-MAZORIo T ZUMBULYADIS, N Pa
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David B. Bailey USI Chemicals Co. 1
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Yvan Boulanger Univ de Montreal Ins
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Helga Cohen Univ of So Carolina Che
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F. David Doty Doty Scientific Inc.
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Alan Freyer Pennsylvania State Univ
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Gordon Hamer Xerox Research Center-
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Timothy Hyman Syracuse University 3
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Robert A Kinsey BF Goodrich 9921Bre
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Jay J. Listinsky U of Rochester-Dep
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Dale Mierke Univ of Calif, San Dieg
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Jeanne C Owens Chemistry Dept., '.1
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Gade S. Reddy DuPont Experimental S
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Charles Schramm Catalytica Assoc. I
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Richard F. Sprecher U.S. Dept of En
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Steve Unger U. C. Davis NMR Facilit
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Toni Wirthlin Varian Associates 611
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th  - 1988 - 51st ENC Conference

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