caa a22 4500 477135803 CHVBK 20180405111717.0 cr unu---uuuuu 170330e19970701xx s 000 0 eng 10.1023/A:1018362914316 doi (NATIONALLICENCE)springer-10.1023/A:1018362914316 Assignments, secondary structure and dynamics of the inhibitor-free catalytic fragment of human fibroblast collagenase [Elektronische Daten] [Franklin Moy, Michael Pisano, Pranab Chanda, Charlotte Urbano, Loran Killar, Mei-Li Sung, Robert Powers] Fibroblast collagenase (MMP-1), a 169-residue protein with amolecular mass of 18.7 kDa, is a matrix metalloproteinase which has beenassociated with pathologies such as arthritis and cancer. The assignments ofthe 1H, 15N, 13CO and13C resonances, determination of the secondary structure andanalysis of 15N relaxation data of the inhibitor-freecatalytic fragment of recombinant human fibroblast collagenase (MMP-1) arepresented. It is shown that MMP-1 is composed of a β-sheet consistingof five β-strands in a mixed parallel and antiparallel arrangement(residues 13-19, 48-53, 59-65, 82-85 and94-99) and three α-helices (residues 27-43, 112-124and 150-160). This is nearly identical to the secondary structuredetermined from the refined X-ray crystal structures of inhibited MMP-1. Themajor difference observed between the NMR solution structure ofinhibitor-free MMP-1 and the X-ray structures of inhibited MMP-1 is thedynamics of the active site. The 2D 15N-1H HSQCspectra, the lack of information in the 15N-edited NOESYspectra, and the generalized order parameters (S2) determinedfrom 15N T1, T2 and NOE datasuggest a slow conformational exchange for residues comprising the activesite (helix B, zinc ligated histidines and the nearby loop region) and ahigh mobility for residues Pro138-Gly144 in thevicinity of the active site for inhibitor-free collagenase. In contrast tothe X-ray structures, only the slow conformational exchange is lost in thepresence of an inhibitor. Kluwer Academic Publishers, 1997 Matrix metalloproteinase nationallicence Collagenase nationallicence Multidimensional NMR nationallicence Resonance assignments nationallicence Secondary structure nationallicence Backbone dynamics nationallicence Moy Franklin Department of Structural Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Pisano Michael Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Chanda Pranab Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Urbano Charlotte Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Killar Loran Department of Endothelial and Cytokine Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Sung Mei-Li Department of Endothelial and Cytokine Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Powers Robert Department of Structural Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut Journal of Biomolecular NMR Kluwer Academic Publishers 10/1(1997-07-01), 9-19 0925-2738 10:1<9 1997 10 10858 https://doi.org/10.1023/A:1018362914316 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1023/A:1018362914316 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Moy Franklin Department of Structural Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Pisano Michael Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Chanda Pranab Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Urbano Charlotte Department of Core Biotechnology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Killar Loran Department of Endothelial and Cytokine Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Sung Mei-Li Department of Endothelial and Cytokine Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 700 1- Powers Robert Department of Structural Biology, Wyeth-Ayerst Research, 10965, Pearl River, NY, U.S.A aut NATIONALLICENCE 773 0- Journal of Biomolecular NMR Kluwer Academic Publishers 10/1(1997-07-01), 9-19 0925-2738 10:1<9 1997 10 10858 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer