Report No xxxx - Instytut Fizyki JÄdrowej PAN

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STUDIES ON CYTOCHROME C UNFOLDING PROCESS USING ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY. QUALIFICATION OF PROXYL-MTS SPIN LABEL IN EXAMINATION OF PROTEIN STRUCTURE Przemysław Grudnik + , Janusz Pyka, Bohdan Turyna, Ryszard Gurbiel, Wojciech Froncisz Department of Biophysics, Faculty of Biotechnology, Jagiellonian University, ul. Gronostajowa 7, 30-387 Kraków, Poland Yeast iso-1-cytochrome c was labeled by two different spin labels: MTSL ((1-Oxyl-2,2,5,5- tetramethyl-∆ 3 -pyrrolin-3-yl) methanethiosulfonate)) and proxyl-MTS ((1-oxyl-2,2,5,5- tetramethylpyrrolidin-3-yl) methyl methanethiosulfonate). Proteins were denaturized in guanidinium hydrochloride. EPR spectroscopy was used to qualify protein unfolding degree. Continuous wave (CW) EPR spectrum of cytochromes c was registered in different concentration of guanidinium hydrochloride. Comparison of our results shows that proxyl- MTS spin label influence on protein structure stability has comparable grade like influence of MTSL spin label. + pgrudnik@op.pl 110
STRUCTURE OF 4-QUINOLINONES ANALYSED BY NMR STUDY AND X-RAY DATA Andrzej Zięba a , Andrzej Maślankiewicz a , Jerzy Sitkowski b , Bohdan Kamieński c , Kinga Suwińska d a Department of Organic Chemistry, The Medical University of Silesia, Jagiellońska 4, 41-200 Sosnowiec; b Institute of Drugs, 30/34 Chełmska, 00-725 Warsaw; c Institute of Organic Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw; d Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw The previous study on 1-ethyl-3-methylthio-4(1H)-quinolinethione 1 and 1-methyl- 4(1H)-pyridinethione 2 performed with the use of 14 N NMR spectroscopy (in CDCl 3 solution) and with X-ray examination led us to the conclusion that the compounds 1 and 2 do not exist in the form of azinethiones, but they exist as 1-alkylazinium-4-thiolates 4 or 5. 1,2 O _ O N R N R + 14 N NMR spectral data (in CDCl 3 solution) of 1-methyl-4(1H)-quinolinone 3 reveals nitrogen atom signal (δ=-220 ppm) with half-height of linewidths ∆v 1/2 =286 Hz. It suggests for pyridinium-type resonance form 4 as the major contributor to the real molecular structure of 3. X-ray examination of 3 shows the planarity of pyridine ring in 3 including the planarity around the endocyclic-nitrogen indicating for sp 2 hybridization of nitrogen N 1 . Planar tricoordinated nitrogen should bear a positive charge, and pyridinium-type resonance form 4 should be major contributor to the real molecular structure of 3. The same structural features of pyridine unit (as concluded from CCDB) were observed also in the case of numerous compounds with 4-quinolinone formula including potent antibacterial drugs. The 1 H, 13 C, 15 N NMR study in the solid state and the solution of 3 in DMSO and those of ciprofloxacine confirmed the mentioned above conclusion. 1. A.Maślankiewicz, A.Zięba, K.Suwińska, J.Chem.Crystallogr., 28, 701 (1998). 2. A.Zięba, A.Maślankiewicz, K.Suwińska, Acta Crystallogr., C58, 32 (2002). 3. A.Zięba, A.Maślankiewicz, V.Milata, J.Sitkowski, Magn. Reson. Chem., 41, 639, (2003) 111
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The Henryk Niewodniczański INSTITU
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Contents R. Banyś, A. Słowik, M.
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J. Kolmas, M. Uniczko, E. Kalinowsk
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Ł. Popenda, Z. Gdaniec, G. Dominia
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USEFULNESS OF PROTON MAGNETIC RESON
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INFLUENCE OF PARAMAGNETIC IONS ON F
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NMR RELAXATION OF PAPER SAMPLES Bar
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SPIN-LATTICE RELAXATION OF D 2 QUAN
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INVESTIGATION OF NEUROPROTECTING EF
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OPTICAL PUMPING OF 3 He Katarzyna C
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NMR STUDY OF GELATION PROCESS OF LO
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MRI INVESTIGATIONS OF HYDROGEL FORM
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CHEMICAL SHIFT TITRATION AT THE INT
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LOCAL DYNAMICS AND ORGANIZATION OF
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1 H NMR DETECTION OF σ-ADDUCTS IN
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HYDRATION OF WHEAT PHOTOSYNTHETIC M
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References: 1. H. Harańczyk On wat
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(EDV) and end-systolic (ESV) volume
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THE MOST STABLE POLYMORPHIC FORM OF
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A DETERMINATION OF ABSOLUTE SHIELDI
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DIAGNOTIC VALUE OF MRI IN CONVERSIO
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NMR AND FTIR STUDY OF MOLECULAR DYN
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EFFECTS OF INTERMOLECULAR INTERACTI
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600000 Integral of 1D MRI profils [
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simultaneous analyse of the tempera
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1 H NMR STUDIES OF PLATINUM(II) CHL
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35 Cl-NQR STUDY OF ELECTRONIC STRUC
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35 Cl- NQR AND 1 H-NMR STUDY OF MOL
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THE SYNTHESIS AND NMR ANALYSIS OF T
Page 59 and 60: STUDY OF MOTIONAL PROCESSES OF DRAW
Page 61 and 62: intensity (arb. units) 0,20 0,15 0,
Page 63 and 64: data for Cβ-nonplanar model 3 are
Page 65 and 66: T 1 DISPERSION AND SELF-DIFFUSION N
Page 67 and 68: A LOW FIELD MRI SYSTEM FOR HYPERPOL
Page 69 and 70: 1 H MAS NMR OF FLAVONOIDS Katarzyna
Page 71 and 72: EFFECT OF TEMPERATURE ON LIPOSOME S
Page 73 and 74: 1 H, 13 C NMR AND GIAO/DFT CALCULAT
Page 75 and 76: NMR STUDY OF THE HUMIC ACIDS EXTRAC
Page 77 and 78: NMR STUDY OF LAYERED ANGANITE La 1.
Page 79 and 80: MAGNETIC SUSCEPTIBILITY EVALUATION
Page 81 and 82: A NOVEL SOURCE OF MAGNETIC FIELD FO
Page 83 and 84: DETERMINATION OF AMINO ACIDS IN BOD
Page 85 and 86: MOLECULAR DYNAMICS OF TERT-BUTYL CH
Page 87 and 88: MR MICROSCOPY IN COMPARISON OF YOUN
Page 89 and 90: NH CH CH 2 NH CH CO COONa n CH 2 m
Page 91 and 92: 35 Cl-NQR STUDY OF MOLECULAR DYNAMI
Page 93 and 94: 35 Cl-NQR STUDY OF THE SUBSTITUENT
Page 95 and 96: 13 C AND 1 H NUCLEAR MAGNETIC SHIEL
Page 97 and 98: 13 C CPMAS NMR OF ANTHOCYANINS AND
Page 99 and 100: INVESTIGATION OF TRANSESTERIFICATIO
Page 101 and 102: T 2 RELAXATION MAP OF ARTICULAR CAR
Page 103 and 104: MICROTOMOGRAPHY STUDIES OF TABLETS
Page 105 and 106: MAPPING OF THE BI-EXPONENTIAL DIFFU
Page 107 and 108: DEUTERIUM NMR IN RMn 2 D 2 (R = Y,
Page 109: The neutron scattering (IINS, QNS,
Page 113: NMR MULTIPOLE RELAXATION IN THE ROT
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Report No xxxx - Instytut Fizyki JÄdrowej PAN