HEADER    HYDROLASE                               14-DEC-16   5MOO              
TITLE     JOINT X-RAY/NEUTRON STRUCTURE OF CATIONIC TRYPSIN IN COMPLEX WITH     
TITLE    2 ANILINE                                                              
COMPND    MOL_ID: 1;                                                            
COMPND   2 MOLECULE: CATIONIC TRYPSIN;                                          
COMPND   3 CHAIN: A;                                                            
COMPND   4 SYNONYM: BETA-TRYPSIN;                                               
COMPND   5 EC: 3.4.21.4                                                         
SOURCE    MOL_ID: 1;                                                            
SOURCE   2 ORGANISM_SCIENTIFIC: BOS TAURUS;                                     
SOURCE   3 ORGANISM_COMMON: BOVINE;                                             
SOURCE   4 ORGANISM_TAXID: 9913                                                 
KEYWDS    HYDROGEN BONDING, PROTONATION, PROTEIN-LIGAND INTERACTION, HYDROLASE  
EXPDTA    X-RAY DIFFRACTION; NEUTRON DIFFRACTION                                
AUTHOR    J.SCHIEBEL,T.E.SCHRADER,A.OSTERMANN,A.HEINE,G.KLEBE                   
REVDAT   3   14-NOV-18 5MOO    1       REMARK                                   
REVDAT   2   23-AUG-17 5MOO    1       ATOM                                     
REVDAT   1   24-MAY-17 5MOO    0                                                
JRNL        AUTH   J.SCHIEBEL,R.GASPARI,A.SANDNER,K.NGO,H.D.GERBER,A.CAVALLI,   
JRNL        AUTH 2 A.OSTERMANN,A.HEINE,G.KLEBE                                  
JRNL        TITL   CHARGES SHIFT PROTONATION: NEUTRON DIFFRACTION REVEALS THAT  
JRNL        TITL 2 ANILINE AND 2-AMINOPYRIDINE BECOME PROTONATED UPON BINDING   
JRNL        TITL 3 TO TRYPSIN.                                                  
JRNL        REF    ANGEW. CHEM. INT. ED. ENGL.   V.  56  4887 2017              
JRNL        REFN                   ESSN 1521-3773                               
JRNL        PMID   28371253                                                     
JRNL        DOI    10.1002/ANIE.201701038                                       
REMARK   2                                                                      
REMARK   2 RESOLUTION.    1.44 ANGSTROMS.                                       
REMARK   3                                                                      
REMARK   3 REFINEMENT.                                                          
REMARK   3   PROGRAM     : PHENIX (DEV_2429)                                    
REMARK   3   AUTHORS     : PAUL ADAMS,PAVEL AFONINE,VINCENT CHEN,IAN            
REMARK   3               : DAVIS,KRESHNA GOPAL,RALF GROSSE-KUNSTLEVE,           
REMARK   3               : LI-WEI HUNG,ROBERT IMMORMINO,TOM IOERGER,            
REMARK   3               : AIRLIE MCCOY,ERIK MCKEE,NIGEL MORIARTY,              
REMARK   3               : REETAL PAI,RANDY READ,JANE RICHARDSON,               
REMARK   3               : DAVID RICHARDSON,TOD ROMO,JIM SACCHETTINI,           
REMARK   3               : NICHOLAS SAUTER,JACOB SMITH,LAURENT                  
REMARK   3               : STORONI,TOM TERWILLIGER,PETER ZWART                  
REMARK   3  X-RAY DATA.                                                         
REMARK   3                                                                      
REMARK   3    REFINEMENT TARGET : NULL                                          
REMARK   3                                                                      
REMARK   3  DATA USED IN REFINEMENT.                                            
REMARK   3   RESOLUTION RANGE HIGH (ANGSTROMS) : 1.44                           
REMARK   3   RESOLUTION RANGE LOW  (ANGSTROMS) : 44.18                          
REMARK   3   MIN(FOBS/SIGMA_FOBS)              : 1.360                          
REMARK   3   COMPLETENESS FOR RANGE        (%) : 97.3                           
REMARK   3   NUMBER OF REFLECTIONS             : 38776                          
REMARK   3                                                                      
REMARK   3  FIT TO DATA USED IN REFINEMENT.                                     
REMARK   3   R VALUE     (WORKING + TEST SET) : 0.136                           
REMARK   3   R VALUE            (WORKING SET) : 0.134                           
REMARK   3   FREE R VALUE                     : 0.160                           
REMARK   3   FREE R VALUE TEST SET SIZE   (%) : 5.050                           
REMARK   3   FREE R VALUE TEST SET COUNT      : 1959                            
REMARK   3                                                                      
REMARK   3  FIT TO DATA USED IN REFINEMENT (IN BINS).                           
REMARK   3   BIN  RESOLUTION RANGE  COMPL.    NWORK NFREE   RWORK  RFREE        
REMARK   3     1 44.2047 -  3.4736    0.99     2867   137  0.1142 0.1105        
REMARK   3     2  3.4736 -  2.7572    1.00     2785   123  0.1260 0.1475        
REMARK   3     3  2.7572 -  2.4087    1.00     2748   140  0.1135 0.1378        
REMARK   3     4  2.4087 -  2.1885    1.00     2716   133  0.0909 0.1214        
REMARK   3     5  2.1885 -  2.0317    1.00     2694   146  0.0856 0.1054        
REMARK   3     6  2.0317 -  1.9119    1.00     2675   155  0.0809 0.1162        
REMARK   3     7  1.9119 -  1.8161    1.00     2678   147  0.0804 0.1144        
REMARK   3     8  1.8161 -  1.7371    1.00     2687   154  0.0772 0.1196        
REMARK   3     9  1.7371 -  1.6702    1.00     2659   125  0.0737 0.1000        
REMARK   3    10  1.6702 -  1.6126    1.00     2661   140  0.0838 0.1455        
REMARK   3    11  1.6126 -  1.5621    0.99     2650   158  0.1086 0.1622        
REMARK   3    12  1.5621 -  1.5175    0.98     2598   135  0.2152 0.2612        
REMARK   3    13  1.5175 -  1.4775    0.98     2614   152  0.2930 0.2871        
REMARK   3    14  1.4775 -  1.4415    0.68     1785   114  0.6638 0.6601        
REMARK   3                                                                      
REMARK   3  BULK SOLVENT MODELLING.                                             
REMARK   3   METHOD USED        : NULL                                          
REMARK   3   SOLVENT RADIUS     : 1.11                                          
REMARK   3   SHRINKAGE RADIUS   : 0.90                                          
REMARK   3   K_SOL              : NULL                                          
REMARK   3   B_SOL              : NULL                                          
REMARK   3                                                                      
REMARK   3  ERROR ESTIMATES.                                                    
REMARK   3   COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED)     : 0.250            
REMARK   3   PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 17.110           
REMARK   3                                                                      
REMARK   3  B VALUES.                                                           
REMARK   3   FROM WILSON PLOT           (A**2) : NULL                           
REMARK   3   MEAN B VALUE      (OVERALL, A**2) : NULL                           
REMARK   3   OVERALL ANISOTROPIC B VALUE.                                       
REMARK   3    B11 (A**2) : NULL                                                 
REMARK   3    B22 (A**2) : NULL                                                 
REMARK   3    B33 (A**2) : NULL                                                 
REMARK   3    B12 (A**2) : NULL                                                 
REMARK   3    B13 (A**2) : NULL                                                 
REMARK   3    B23 (A**2) : NULL                                                 
REMARK   3                                                                      
REMARK   3  TWINNING INFORMATION.                                               
REMARK   3   FRACTION: NULL                                                     
REMARK   3   OPERATOR: NULL                                                     
REMARK   3                                                                      
REMARK   3  DEVIATIONS FROM IDEAL VALUES.                                       
REMARK   3                 RMSD          COUNT                                  
REMARK   3   BOND      :  0.006           3758                                  
REMARK   3   ANGLE     :  1.085           6417                                  
REMARK   3   CHIRALITY :  0.093            270                                  
REMARK   3   PLANARITY :  0.006            790                                  
REMARK   3   DIHEDRAL  : 12.911            976                                  
REMARK   3                                                                      
REMARK   3  TLS DETAILS                                                         
REMARK   3   NUMBER OF TLS GROUPS  : NULL                                       
REMARK   3                                                                      
REMARK   3  NCS DETAILS                                                         
REMARK   3   NUMBER OF NCS GROUPS : NULL                                        
REMARK   3                                                                      
REMARK   3  OTHER REFINEMENT REMARKS: NULL                                      
REMARK   3  NEUTRON DATA.                                                       
REMARK   3                                                                      
REMARK   3    REFINEMENT TARGET : NULL                                          
REMARK   3                                                                      
REMARK   3  DATA USED IN REFINEMENT.                                            
REMARK   3   RESOLUTION RANGE HIGH (ANGSTROMS) : 1.43                           
REMARK   3   RESOLUTION RANGE LOW  (ANGSTROMS) : 22.09                          
REMARK   3   MIN(FOBS/SIGMA_FOBS)              : NULL                           
REMARK   3   COMPLETENESS FOR RANGE        (%) : 93.8                           
REMARK   3   NUMBER OF REFLECTIONS             : 38317                          
REMARK   3                                                                      
REMARK   3  FIT TO DATA USED IN REFINEMENT.                                     
REMARK   3   R VALUE     (WORKING + TEST SET) : 0.171                           
REMARK   3   R VALUE            (WORKING SET) : 0.170                           
REMARK   3   FREE R VALUE                     : 0.185                           
REMARK   3   FREE R VALUE TEST SET SIZE   (%) : 4.990                           
REMARK   3   FREE R VALUE TEST SET COUNT      : 1911                            
REMARK   3                                                                      
REMARK   3  FIT TO DATA USED IN REFINEMENT (IN BINS).                           
REMARK   3   BIN  RESOLUTION RANGE  COMPL.    NWORK NFREE   RWORK  RFREE        
REMARK   3     1 22.0946 -  3.4405    0.95     2833   131  0.1462 0.1456        
REMARK   3     2  3.4405 -  2.7324    0.95     2719   123  0.1506 0.1684        
REMARK   3     3  2.7324 -  2.3875    0.96     2682   133  0.1347 0.1460        
REMARK   3     4  2.3875 -  2.1694    0.92     2562   127  0.1378 0.1570        
REMARK   3     5  2.1694 -  2.0140    0.93     2546   136  0.1432 0.1525        
REMARK   3     6  2.0140 -  1.8954    0.93     2553   151  0.1502 0.1687        
REMARK   3     7  1.8954 -  1.8005    0.94     2594   136  0.1693 0.1756        
REMARK   3     8  1.8005 -  1.7221    0.94     2580   132  0.1794 0.1874        
REMARK   3     9  1.7221 -  1.6559    0.95     2622   136  0.1837 0.2125        
REMARK   3    10  1.6559 -  1.5987    0.96     2635   138  0.1969 0.2123        
REMARK   3    11  1.5987 -  1.5488    0.96     2628   145  0.2224 0.2350        
REMARK   3    12  1.5488 -  1.5045    0.97     2617   150  0.2601 0.2667        
REMARK   3    13  1.5045 -  1.4649    0.95     2569   150  0.2488 0.2986        
REMARK   3    14  1.4649 -  1.4292    0.84     2266   123  0.2666 0.2866        
REMARK   3                                                                      
REMARK   3  BULK SOLVENT MODELLING.                                             
REMARK   3   METHOD USED        : NULL                                          
REMARK   3   SOLVENT RADIUS     : 1.11                                          
REMARK   3   SHRINKAGE RADIUS   : 0.90                                          
REMARK   3   K_SOL              : NULL                                          
REMARK   3   B_SOL              : NULL                                          
REMARK   3                                                                      
REMARK   3  ERROR ESTIMATES.                                                    
REMARK   3   COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED)     : 0.250            
REMARK   3   PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 17.110           
REMARK   3                                                                      
REMARK   3  B VALUES.                                                           
REMARK   3   FROM WILSON PLOT           (A**2) : NULL                           
REMARK   3   MEAN B VALUE      (OVERALL, A**2) : NULL                           
REMARK   3   OVERALL ANISOTROPIC B VALUE.                                       
REMARK   3    B11 (A**2) : NULL                                                 
REMARK   3    B22 (A**2) : NULL                                                 
REMARK   3    B33 (A**2) : NULL                                                 
REMARK   3    B12 (A**2) : NULL                                                 
REMARK   3    B13 (A**2) : NULL                                                 
REMARK   3    B23 (A**2) : NULL                                                 
REMARK   3                                                                      
REMARK   3  TWINNING INFORMATION.                                               
REMARK   3   FRACTION: NULL                                                     
REMARK   3   OPERATOR: NULL                                                     
REMARK   3                                                                      
REMARK   3  DEVIATIONS FROM IDEAL VALUES.                                       
REMARK   3                 RMSD          COUNT                                  
REMARK   3   BOND      :  0.006           3758                                  
REMARK   3   ANGLE     :  1.085           6417                                  
REMARK   3   CHIRALITY :  0.093            270                                  
REMARK   3   PLANARITY :  0.006            790                                  
REMARK   3   DIHEDRAL  : 12.911            976                                  
REMARK   3                                                                      
REMARK   3  TLS DETAILS                                                         
REMARK   3   NUMBER OF TLS GROUPS  : NULL                                       
REMARK   3                                                                      
REMARK   3  NCS DETAILS                                                         
REMARK   3   NUMBER OF NCS GROUPS : NULL                                        
REMARK   3                                                                      
REMARK   3  OTHER REFINEMENT REMARKS: NULL                                      
REMARK   4                                                                      
REMARK   4 5MOO COMPLIES WITH FORMAT V. 3.30, 13-JUL-11                         
REMARK 100                                                                      
REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY PDBE ON 14-DEC-16.                  
REMARK 100 THE DEPOSITION ID IS D_1200002723.                                   
REMARK 200                                                                      
REMARK 200 EXPERIMENTAL DETAILS                                                 
REMARK 200  EXPERIMENT TYPE                : X-RAY DIFFRACTION                  
REMARK 200  DATE OF DATA COLLECTION        : 19-FEB-16                          
REMARK 200  TEMPERATURE           (KELVIN) : 295                                
REMARK 200  PH                             : 7.5                                
REMARK 200  NUMBER OF CRYSTALS USED        : 1                                  
REMARK 200                                                                      
REMARK 200  SYNCHROTRON              (Y/N) : N                                  
REMARK 200  RADIATION SOURCE               : SEALED TUBE                        
REMARK 200  BEAMLINE                       : NULL                               
REMARK 200  X-RAY GENERATOR MODEL          : OTHER                              
REMARK 200  MONOCHROMATIC OR LAUE    (M/L) : M                                  
REMARK 200  WAVELENGTH OR RANGE        (A) : 1.54179                            
REMARK 200  MONOCHROMATOR                  : NULL                               
REMARK 200  OPTICS                         : NULL                               
REMARK 200                                                                      
REMARK 200  DETECTOR TYPE                  : IMAGE PLATE                        
REMARK 200  DETECTOR MANUFACTURER          : MAR SCANNER 345 MM PLATE           
REMARK 200  INTENSITY-INTEGRATION SOFTWARE : NULL                               
REMARK 200  DATA SCALING SOFTWARE          : NULL                               
REMARK 200                                                                      
REMARK 200  NUMBER OF UNIQUE REFLECTIONS   : 38793                              
REMARK 200  RESOLUTION RANGE HIGH      (A) : 1.441                              
REMARK 200  RESOLUTION RANGE LOW       (A) : 44.184                             
REMARK 200  REJECTION CRITERIA  (SIGMA(I)) : NULL                               
REMARK 200                                                                      
REMARK 200 OVERALL.                                                             
REMARK 200  COMPLETENESS FOR RANGE     (%) : 97.3                               
REMARK 200  DATA REDUNDANCY                : 7.361                              
REMARK 200  R MERGE                    (I) : 0.04500                            
REMARK 200  R SYM                      (I) : NULL                               
REMARK 200  <I/SIGMA(I)> FOR THE DATA SET  : 27.0100                            
REMARK 200                                                                      
REMARK 200 IN THE HIGHEST RESOLUTION SHELL.                                     
REMARK 200  HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.44                     
REMARK 200  HIGHEST RESOLUTION SHELL, RANGE LOW  (A) : 1.53                     
REMARK 200  COMPLETENESS FOR SHELL     (%) : 84.6                               
REMARK 200  DATA REDUNDANCY IN SHELL       : 6.03                               
REMARK 200  R MERGE FOR SHELL          (I) : 0.22900                            
REMARK 200  R SYM FOR SHELL            (I) : NULL                               
REMARK 200  <I/SIGMA(I)> FOR SHELL         : 9.860                              
REMARK 200                                                                      
REMARK 200 DIFFRACTION PROTOCOL: SINGLE WAVELENGTH                              
REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: MOLECULAR REPLACEMENT        
REMARK 200 SOFTWARE USED: PHASER                                                
REMARK 200 STARTING MODEL: 4I8H                                                 
REMARK 200                                                                      
REMARK 200 REMARK: NULL                                                         
REMARK 230                                                                      
REMARK 230 EXPERIMENTAL DETAILS                                                 
REMARK 230  EXPERIMENT TYPE                : NEUTRON DIFFRACTION                
REMARK 230  DATE OF DATA COLLECTION        : 22-JUL-16                          
REMARK 230  TEMPERATURE           (KELVIN) : 295.0                              
REMARK 230  PH                             : 7.50                               
REMARK 230  NUMBER OF CRYSTALS USED        : NULL                               
REMARK 230                                                                      
REMARK 230  NEUTRON SOURCE                 : NUCLEAR REACTOR                    
REMARK 230  BEAMLINE                       : BIODIFF                            
REMARK 230  WAVELENGTH OR RANGE        (A) : 2.667                              
REMARK 230  MONOCHROMATOR                  : NULL                               
REMARK 230  OPTICS                         : NULL                               
REMARK 230                                                                      
REMARK 230  DETECTOR TYPE                  : IMAGE PLATE                        
REMARK 230  DETECTOR MANUFACTURER          : MAATEL BIODIFF                     
REMARK 230  INTENSITY-INTEGRATION SOFTWARE : XDS, HKL-2000                      
REMARK 230  DATA SCALING SOFTWARE          : XDS, HKL-2000                      
REMARK 230                                                                      
REMARK 230  NUMBER OF UNIQUE REFLECTIONS   : 38342                              
REMARK 230  RESOLUTION RANGE HIGH      (A) : 1.430                              
REMARK 230  RESOLUTION RANGE LOW       (A) : 50.000                             
REMARK 230  REJECTION CRITERIA  (SIGMA(I)) : NULL                               
REMARK 230                                                                      
REMARK 230 OVERALL.                                                             
REMARK 230  COMPLETENESS FOR RANGE     (%) : 93.8                               
REMARK 230  DATA REDUNDANCY                : 2.500                              
REMARK 230  R MERGE                    (I) : 0.09800                            
REMARK 230  R SYM                      (I) : NULL                               
REMARK 230  <I/SIGMA(I)> FOR THE DATA SET  : 7.2530                             
REMARK 230                                                                      
REMARK 230 IN THE HIGHEST RESOLUTION SHELL.                                     
REMARK 230  HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.43                     
REMARK 230  HIGHEST RESOLUTION SHELL, RANGE LOW  (A) : 1.45                     
REMARK 230  COMPLETENESS FOR SHELL     (%) : 82.1                               
REMARK 230  DATA REDUNDANCY IN SHELL       : 1.60                               
REMARK 230  R MERGE FOR SHELL          (I) : 0.38700                            
REMARK 230  R SYM FOR SHELL            (I) : NULL                               
REMARK 230  <I/SIGMA(I)> FOR SHELL         : 1.858                              
REMARK 230                                                                      
REMARK 230 METHOD USED TO DETERMINE THE STRUCTURE: MOLECULAR REPLACEMENT        
REMARK 230 SOFTWARE USED : PHASER                                               
REMARK 230 STARTING MODEL: 4I8H                                                 
REMARK 230                                                                      
REMARK 230 REMARK: NULL                                                         
REMARK 280                                                                      
REMARK 280 CRYSTAL                                                              
REMARK 280 SOLVENT CONTENT, VS   (%): 46.98                                     
REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.32                     
REMARK 280                                                                      
REMARK 280 CRYSTALLIZATION CONDITIONS: 0.2 M AMMONIUM SULFATE, 0.1 M HEPES PH   
REMARK 280  7.5, 16.5-17.0% (W/V) PEG 8000, VAPOR DIFFUSION, SITTING DROP,      
REMARK 280  TEMPERATURE 277K                                                    
REMARK 290                                                                      
REMARK 290 CRYSTALLOGRAPHIC SYMMETRY                                            
REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 21 21 21                       
REMARK 290                                                                      
REMARK 290      SYMOP   SYMMETRY                                                
REMARK 290     NNNMMM   OPERATOR                                                
REMARK 290       1555   X,Y,Z                                                   
REMARK 290       2555   -X+1/2,-Y,Z+1/2                                         
REMARK 290       3555   -X,Y+1/2,-Z+1/2                                         
REMARK 290       4555   X+1/2,-Y+1/2,-Z                                         
REMARK 290                                                                      
REMARK 290     WHERE NNN -> OPERATOR NUMBER                                     
REMARK 290           MMM -> TRANSLATION VECTOR                                  
REMARK 290                                                                      
REMARK 290 CRYSTALLOGRAPHIC SYMMETRY TRANSFORMATIONS                            
REMARK 290 THE FOLLOWING TRANSFORMATIONS OPERATE ON THE ATOM/HETATM             
REMARK 290 RECORDS IN THIS ENTRY TO PRODUCE CRYSTALLOGRAPHICALLY                
REMARK 290 RELATED MOLECULES.                                                   
REMARK 290   SMTRY1   1  1.000000  0.000000  0.000000        0.00000            
REMARK 290   SMTRY2   1  0.000000  1.000000  0.000000        0.00000            
REMARK 290   SMTRY3   1  0.000000  0.000000  1.000000        0.00000            
REMARK 290   SMTRY1   2 -1.000000  0.000000  0.000000       27.43750            
REMARK 290   SMTRY2   2  0.000000 -1.000000  0.000000        0.00000            
REMARK 290   SMTRY3   2  0.000000  0.000000  1.000000       33.72900            
REMARK 290   SMTRY1   3 -1.000000  0.000000  0.000000        0.00000            
REMARK 290   SMTRY2   3  0.000000  1.000000  0.000000       29.23600            
REMARK 290   SMTRY3   3  0.000000  0.000000 -1.000000       33.72900            
REMARK 290   SMTRY1   4  1.000000  0.000000  0.000000       27.43750            
REMARK 290   SMTRY2   4  0.000000 -1.000000  0.000000       29.23600            
REMARK 290   SMTRY3   4  0.000000  0.000000 -1.000000        0.00000            
REMARK 290                                                                      
REMARK 290 REMARK: NULL                                                         
REMARK 300                                                                      
REMARK 300 BIOMOLECULE: 1                                                       
REMARK 300 SEE REMARK 350 FOR THE AUTHOR PROVIDED AND/OR PROGRAM                
REMARK 300 GENERATED ASSEMBLY INFORMATION FOR THE STRUCTURE IN                  
REMARK 300 THIS ENTRY. THE REMARK MAY ALSO PROVIDE INFORMATION ON               
REMARK 300 BURIED SURFACE AREA.                                                 
REMARK 350                                                                      
REMARK 350 COORDINATES FOR A COMPLETE MULTIMER REPRESENTING THE KNOWN           
REMARK 350 BIOLOGICALLY SIGNIFICANT OLIGOMERIZATION STATE OF THE                
REMARK 350 MOLECULE CAN BE GENERATED BY APPLYING BIOMT TRANSFORMATIONS          
REMARK 350 GIVEN BELOW.  BOTH NON-CRYSTALLOGRAPHIC AND                          
REMARK 350 CRYSTALLOGRAPHIC OPERATIONS ARE GIVEN.                               
REMARK 350                                                                      
REMARK 350 BIOMOLECULE: 1                                                       
REMARK 350 AUTHOR DETERMINED BIOLOGICAL UNIT: MONOMERIC                         
REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: MONOMERIC                  
REMARK 350 SOFTWARE USED: PISA                                                  
REMARK 350 TOTAL BURIED SURFACE AREA: 17960 ANGSTROM**2                         
REMARK 350 SURFACE AREA OF THE COMPLEX: 8900 ANGSTROM**2                        
REMARK 350 CHANGE IN SOLVENT FREE ENERGY: 19.0 KCAL/MOL                         
REMARK 350 APPLY THE FOLLOWING TO CHAINS: A                                     
REMARK 350   BIOMT1   1  1.000000  0.000000  0.000000        0.00000            
REMARK 350   BIOMT2   1  0.000000  1.000000  0.000000        0.00000            
REMARK 350   BIOMT3   1  0.000000  0.000000  1.000000        0.00000            
REMARK 470                                                                      
REMARK 470 MISSING ATOM                                                         
REMARK 470 THE FOLLOWING RESIDUES HAVE MISSING ATOMS (M=MODEL NUMBER;           
REMARK 470 RES=RESIDUE NAME; C=CHAIN IDENTIFIER; SSEQ=SEQUENCE NUMBER;          
REMARK 470 I=INSERTION CODE):                                                   
REMARK 470   M RES CSSEQI  ATOMS                                                
REMARK 470     LYS A 109    CD   CE   NZ                                        
REMARK 470     LYS A 145    CE   NZ                                             
REMARK 470     SER A 147    OG                                                  
REMARK 470     LYS A 188A   NZ                                                  
REMARK 470     GLN A 192    CG   CD   OE1  NE2                                  
REMARK 470     LYS A 222    CD   CE   NZ                                        
REMARK 470     LYS A 239    CE   NZ                                             
REMARK 470     GLN A 240    CD   OE1  NE2                                       
REMARK 500                                                                      
REMARK 500 GEOMETRY AND STEREOCHEMISTRY                                         
REMARK 500 SUBTOPIC: CLOSE CONTACTS IN SAME ASYMMETRIC UNIT                     
REMARK 500                                                                      
REMARK 500 THE FOLLOWING ATOMS ARE IN CLOSE CONTACT.                            
REMARK 500                                                                      
REMARK 500  ATM1  RES C  SSEQI   ATM2  RES C  SSEQI           DISTANCE          
REMARK 500   OE1  GLU A    77     D1   DOD A   401              1.60            
REMARK 500                                                                      
REMARK 500 REMARK: NULL                                                         
REMARK 500                                                                      
REMARK 500 GEOMETRY AND STEREOCHEMISTRY                                         
REMARK 500 SUBTOPIC: CLOSE CONTACTS                                             
REMARK 500                                                                      
REMARK 500 THE FOLLOWING ATOMS THAT ARE RELATED BY CRYSTALLOGRAPHIC             
REMARK 500 SYMMETRY ARE IN CLOSE CONTACT.  AN ATOM LOCATED WITHIN 0.15          
REMARK 500 ANGSTROMS OF A SYMMETRY RELATED ATOM IS ASSUMED TO BE ON A           
REMARK 500 SPECIAL POSITION AND IS, THEREFORE, LISTED IN REMARK 375             
REMARK 500 INSTEAD OF REMARK 500.  ATOMS WITH NON-BLANK ALTERNATE               
REMARK 500 LOCATION INDICATORS ARE NOT INCLUDED IN THE CALCULATIONS.            
REMARK 500                                                                      
REMARK 500 DISTANCE CUTOFF:                                                     
REMARK 500 2.2 ANGSTROMS FOR CONTACTS NOT INVOLVING HYDROGEN ATOMS              
REMARK 500 1.6 ANGSTROMS FOR CONTACTS INVOLVING HYDROGEN ATOMS                  
REMARK 500                                                                      
REMARK 500  ATM1  RES C  SSEQI   ATM2  RES C  SSEQI  SSYMOP   DISTANCE          
REMARK 500   OD1  ASP A   153     D2   DOD A   541     4445     1.57            
REMARK 500                                                                      
REMARK 500 REMARK: NULL                                                         
REMARK 500                                                                      
REMARK 500 GEOMETRY AND STEREOCHEMISTRY                                         
REMARK 500 SUBTOPIC: TORSION ANGLES                                             
REMARK 500                                                                      
REMARK 500 TORSION ANGLES OUTSIDE THE EXPECTED RAMACHANDRAN REGIONS:            
REMARK 500 (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN IDENTIFIER;               
REMARK 500 SSEQ=SEQUENCE NUMBER; I=INSERTION CODE).                             
REMARK 500                                                                      
REMARK 500 STANDARD TABLE:                                                      
REMARK 500 FORMAT:(10X,I3,1X,A3,1X,A1,I4,A1,4X,F7.2,3X,F7.2)                    
REMARK 500                                                                      
REMARK 500 EXPECTED VALUES: GJ KLEYWEGT AND TA JONES (1996). PHI/PSI-           
REMARK 500 CHOLOGY: RAMACHANDRAN REVISITED. STRUCTURE 4, 1395 - 1400            
REMARK 500                                                                      
REMARK 500  M RES CSSEQI        PSI       PHI                                   
REMARK 500    ASP A  71      -76.38   -121.77                                   
REMARK 500                                                                      
REMARK 500 REMARK: NULL                                                         
REMARK 620                                                                      
REMARK 620 METAL COORDINATION                                                   
REMARK 620 (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN IDENTIFIER;               
REMARK 620 SSEQ=SEQUENCE NUMBER; I=INSERTION CODE):                             
REMARK 620                                                                      
REMARK 620 COORDINATION ANGLES FOR:  M RES CSSEQI METAL                         
REMARK 620                              CA A 301  CA                            
REMARK 620 N RES CSSEQI ATOM                                                    
REMARK 620 1 GLU A  70   OE1                                                    
REMARK 620 2 ASN A  72   O    90.2                                              
REMARK 620 3 VAL A  75   O   164.0  81.6                                        
REMARK 620 4 GLU A  80   OE2 102.6 160.6  89.1                                  
REMARK 620 5 DOD A 401   O    87.4  87.9 105.9  78.3                            
REMARK 620 6 DOD A 443   O    80.2 103.0  88.2  93.6 163.4                      
REMARK 620 N                    1     2     3     4     5                       
REMARK 800                                                                      
REMARK 800 SITE                                                                 
REMARK 800 SITE_IDENTIFIER: AC1                                                 
REMARK 800 EVIDENCE_CODE: SOFTWARE                                              
REMARK 800 SITE_DESCRIPTION: binding site for residue CA A 301                  
REMARK 800                                                                      
REMARK 800 SITE_IDENTIFIER: AC2                                                 
REMARK 800 EVIDENCE_CODE: SOFTWARE                                              
REMARK 800 SITE_DESCRIPTION: binding site for residue WOT A 302                 
REMARK 800                                                                      
REMARK 800 SITE_IDENTIFIER: AC3                                                 
REMARK 800 EVIDENCE_CODE: SOFTWARE                                              
REMARK 800 SITE_DESCRIPTION: binding site for residue SO4 A 303                 
REMARK 900                                                                      
REMARK 900 RELATED ENTRIES                                                      
REMARK 900 RELATED ID: 5MNA   RELATED DB: PDB                                   
REMARK 900 REFINEMENT AGAINST ONLY THE X-RAY DIFFRACTION DATA RESULTED IN THIS  
REMARK 900 STRUCTURE                                                            
REMARK 900 RELATED ID: 5MNY   RELATED DB: PDB                                   
REMARK 900 REFINEMENT AGAINST ONLY THE NEUTRON DIFFRACTION DATA RESULTED IN     
REMARK 900 THIS STRUCTURE                                                       
DBREF  5MOO A   16   245  UNP    P00760   TRY1_BOVIN      24    246             
SEQRES   1 A  223  ILE VAL GLY GLY TYR THR CYS GLY ALA ASN THR VAL PRO          
SEQRES   2 A  223  TYR GLN VAL SER LEU ASN SER GLY TYR HIS PHE CYS GLY          
SEQRES   3 A  223  GLY SER LEU ILE ASN SER GLN TRP VAL VAL SER ALA ALA          
SEQRES   4 A  223  HIS CYS TYR LYS SER GLY ILE GLN VAL ARG LEU GLY GLU          
SEQRES   5 A  223  ASP ASN ILE ASN VAL VAL GLU GLY ASN GLU GLN PHE ILE          
SEQRES   6 A  223  SER ALA SER LYS SER ILE VAL HIS PRO SER TYR ASN SER          
SEQRES   7 A  223  ASN THR LEU ASN ASN ASP ILE MET LEU ILE LYS LEU LYS          
SEQRES   8 A  223  SER ALA ALA SER LEU ASN SER ARG VAL ALA SER ILE SER          
SEQRES   9 A  223  LEU PRO THR SER CYS ALA SER ALA GLY THR GLN CYS LEU          
SEQRES  10 A  223  ILE SER GLY TRP GLY ASN THR LYS SER SER GLY THR SER          
SEQRES  11 A  223  TYR PRO ASP VAL LEU LYS CYS LEU LYS ALA PRO ILE LEU          
SEQRES  12 A  223  SER ASP SER SER CYS LYS SER ALA TYR PRO GLY GLN ILE          
SEQRES  13 A  223  THR SER ASN MET PHE CYS ALA GLY TYR LEU GLU GLY GLY          
SEQRES  14 A  223  LYS ASP SER CYS GLN GLY ASP SER GLY GLY PRO VAL VAL          
SEQRES  15 A  223  CYS SER GLY LYS LEU GLN GLY ILE VAL SER TRP GLY SER          
SEQRES  16 A  223  GLY CYS ALA GLN LYS ASN LYS PRO GLY VAL TYR THR LYS          
SEQRES  17 A  223  VAL CYS ASN TYR VAL SER TRP ILE LYS GLN THR ILE ALA          
SEQRES  18 A  223  SER ASN                                                      
HET     CA  A 301       1                                                       
HET    WOT  A 302      11                                                       
HET    SO4  A 303       5                                                       
HETNAM      CA CALCIUM ION                                                      
HETNAM     WOT PHENYLAZANIUM                                                    
HETNAM     SO4 SULFATE ION                                                      
FORMUL   2   CA    CA 2+                                                        
FORMUL   3  WOT    C6 H8 N 1+                                                   
FORMUL   4  SO4    O4 S 2-                                                      
FORMUL   5  DOD   *149(D2 O)                                                    
HELIX    1 AA1 ALA A   55  TYR A   59  5                                   5    
HELIX    2 AA2 SER A  164  TYR A  172  1                                   9    
HELIX    3 AA3 TYR A  234  ASN A  245  1                                  12    
SHEET    1 AA1 7 TYR A  20  THR A  21  0                                        
SHEET    2 AA1 7 LYS A 156  PRO A 161 -1  O  CYS A 157   N  TYR A  20           
SHEET    3 AA1 7 GLN A 135  GLY A 140 -1  N  ILE A 138   O  LEU A 158           
SHEET    4 AA1 7 PRO A 198  CYS A 201 -1  O  VAL A 200   N  LEU A 137           
SHEET    5 AA1 7 LYS A 204  TRP A 215 -1  O  LYS A 204   N  CYS A 201           
SHEET    6 AA1 7 GLY A 226  LYS A 230 -1  O  VAL A 227   N  TRP A 215           
SHEET    7 AA1 7 MET A 180  ALA A 183 -1  N  PHE A 181   O  TYR A 228           
SHEET    1 AA2 7 GLN A  30  ASN A  34  0                                        
SHEET    2 AA2 7 HIS A  40  ASN A  48 -1  O  CYS A  42   N  LEU A  33           
SHEET    3 AA2 7 TRP A  51  SER A  54 -1  O  VAL A  53   N  SER A  45           
SHEET    4 AA2 7 MET A 104  LEU A 108 -1  O  ILE A 106   N  VAL A  52           
SHEET    5 AA2 7 GLN A  81  VAL A  90 -1  N  ILE A  89   O  LEU A 105           
SHEET    6 AA2 7 GLN A  64  LEU A  67 -1  N  LEU A  67   O  GLN A  81           
SHEET    7 AA2 7 GLN A  30  ASN A  34 -1  N  SER A  32   O  ARG A  66           
SSBOND   1 CYS A   22    CYS A  157                          1555   1555  2.03  
SSBOND   2 CYS A   42    CYS A   58                          1555   1555  2.04  
SSBOND   3 CYS A  128    CYS A  232                          1555   1555  2.01  
SSBOND   4 CYS A  136    CYS A  201                          1555   1555  2.01  
SSBOND   5 CYS A  168    CYS A  182                          1555   1555  2.02  
SSBOND   6 CYS A  191    CYS A  220                          1555   1555  2.02  
LINK         OE1 GLU A  70                CA    CA A 301     1555   1555  2.23  
LINK         O   ASN A  72                CA    CA A 301     1555   1555  2.32  
LINK         O   VAL A  75                CA    CA A 301     1555   1555  2.27  
LINK         OE2 GLU A  80                CA    CA A 301     1555   1555  2.33  
LINK        CA    CA A 301                 O   DOD A 401     1555   1555  2.37  
LINK        CA    CA A 301                 O   DOD A 443     1555   1555  2.31  
SITE     1 AC1  6 GLU A  70  ASN A  72  VAL A  75  GLU A  80                    
SITE     2 AC1  6 DOD A 401  DOD A 443                                          
SITE     1 AC2  8 ASP A 189  SER A 190  SER A 195  VAL A 213                    
SITE     2 AC2  8 TRP A 215  GLY A 219  DOD A 419  DOD A 486                    
SITE     1 AC3  5 HIS A  57  GLN A 192  GLY A 193  SER A 195                    
SITE     2 AC3  5 DOD A 480                                                     
CRYST1   54.875   58.472   67.458  90.00  90.00  90.00 P 21 21 21    4          
ORIGX1      1.000000  0.000000  0.000000        0.00000                         
ORIGX2      0.000000  1.000000  0.000000        0.00000                         
ORIGX3      0.000000  0.000000  1.000000        0.00000                         
SCALE1      0.018223  0.000000  0.000000        0.00000                         
SCALE2      0.000000  0.017102  0.000000        0.00000                         
SCALE3      0.000000  0.000000  0.014824        0.00000                         
