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HEADER    HYDROLYTIC ENZYME                       14-MAR-96   1DIN
TITLE     DIENELACTONE HYDROLASE AT 2.8 ANGSTROMS
COMPND    MOL_ID: 1;
COMPND   2 MOLECULE: DIENELACTONE HYDROLASE;
COMPND   3 CHAIN: NULL;
COMPND   4 SYNONYM: DLH;
COMPND   5 EC: 3.1.1.45;
COMPND   6 ENGINEERED: YES
SOURCE    MOL_ID: 1;
SOURCE   2 ORGANISM_SCIENTIFIC: PSEUDOMONAS SP.;
SOURCE   3 STRAIN: B13;
SOURCE   4 EXPRESSION_SYSTEM: EXPRESSED UNDER OWN PROMOTER;
SOURCE   5 EXPRESSION_SYSTEM_PLASMID: PDC100;
SOURCE   6 EXPRESSION_SYSTEM_GENE: CLC D
KEYWDS    DIENELACTONE HYDROLASE, AROMATIC HYDROCARBON CATABOLISM,
KEYWDS   2 SERINE ESTERASE, CARBOXYMETHYLENEBUTENOLIDASE,
KEYWDS   3 HYDROLYTIC ENZYME
EXPDTA    X-RAY DIFFRACTION
AUTHOR    D.L.OLLIS,D.PATHAK
REVDAT   1   17-AUG-96 1DIN    0
JRNL        AUTH   D.PATHAK,D.OLLIS
JRNL        TITL   REFINED STRUCTURE OF DIENELACTONE HYDROLASE AT 1.8
JRNL        TITL 2 A
JRNL        REF    J.MOL.BIOL.                   V. 214   497 1990
JRNL        REFN   ASTM JMOBAK  UK ISSN 0022-2836                 0070
REMARK   1
REMARK   1 REFERENCE 1
REMARK   1  AUTH   D.PATHAK,K.L.NGAI,D.OLLIS
REMARK   1  TITL   X-RAY CRYSTALLOGRAPHIC STRUCTURE OF DIENELACTONE
REMARK   1  TITL 2 HYDROLASE AT 2.8 A
REMARK   1  REF    J.MOL.BIOL.                   V. 204   435 1988
REMARK   1  REFN   ASTM JMOBAK  UK ISSN 0022-2836                 0070
REMARK   1 REFERENCE 2
REMARK   1  AUTH   D.L.OLLIS,K.L.NGAI
REMARK   1  TITL   CRYSTALLIZATION AND PRELIMINARY X-RAY
REMARK   1  TITL 2 CRYSTALLOGRAPHIC DATA OF DIENELACTONE HYDROLASE
REMARK   1  TITL 3 FROM PSEUDOMONAS SP. B13
REMARK   1  REF    J.BIOL.CHEM.                  V. 260  9818 1985
REMARK   1  REFN   ASTM JBCHA3  US ISSN 0021-9258                 0071
REMARK   2
REMARK   2 RESOLUTION. 1.8  ANGSTROMS.
REMARK   3
REMARK   3 REFINEMENT.
REMARK   3   PROGRAM     : PROLSQ
REMARK   3   AUTHORS     : KONNERT,HENDRICKSON
REMARK   3
REMARK   3  DATA USED IN REFINEMENT.
REMARK   3   RESOLUTION RANGE HIGH (ANGSTROMS) : 1.8
REMARK   3   RESOLUTION RANGE LOW  (ANGSTROMS) : 10.
REMARK   3   DATA CUTOFF            (SIGMA(F)) : 0.0
REMARK   3   COMPLETENESS FOR RANGE        (%) : 95.
REMARK   3   NUMBER OF REFLECTIONS             : 23835
REMARK   3
REMARK   3  FIT TO DATA USED IN REFINEMENT.
REMARK   3   CROSS-VALIDATION METHOD          : NULL
REMARK   3   FREE R VALUE TEST SET SELECTION  : NULL
REMARK   3   R VALUE     (WORKING + TEST SET) : NULL
REMARK   3   R VALUE            (WORKING SET) : 0.150
REMARK   3   FREE R VALUE                     : NULL
REMARK   3   FREE R VALUE TEST SET SIZE   (%) : NULL
REMARK   3   FREE R VALUE TEST SET COUNT      : NULL
REMARK   3
REMARK   3  FIT/AGREEMENT OF MODEL WITH ALL DATA.
REMARK   3   R VALUE   (WORKING + TEST SET, NO CUTOFF) : NULL
REMARK   3   R VALUE          (WORKING SET, NO CUTOFF) : NULL
REMARK   3   FREE R VALUE                  (NO CUTOFF) : NULL
REMARK   3   FREE R VALUE TEST SET SIZE (%, NO CUTOFF) : NULL
REMARK   3   FREE R VALUE TEST SET COUNT   (NO CUTOFF) : NULL
REMARK   3   TOTAL NUMBER OF REFLECTIONS   (NO CUTOFF) : NULL
REMARK   3
REMARK   3  NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT.
REMARK   3   PROTEIN ATOMS            : 1780
REMARK   3   NUCLEIC ACID ATOMS       : 0
REMARK   3   HETEROGEN ATOMS          : 0
REMARK   3   SOLVENT ATOMS            : 279
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  ESTIMATED COORDINATE ERROR.
REMARK   3   ESD FROM LUZZATI PLOT        (A) : 0.15
REMARK   3   ESD FROM SIGMAA              (A) : NULL
REMARK   3   LOW RESOLUTION CUTOFF        (A) : NULL
REMARK   3
REMARK   3  RMS DEVIATIONS FROM IDEAL VALUES.
REMARK   3   DISTANCE RESTRAINTS.                    RMS    SIGMA
REMARK   3    BOND LENGTH                     (A) : 0.014 ; 0.010
REMARK   3    ANGLE DISTANCE                  (A) : NULL  ; NULL
REMARK   3    INTRAPLANAR 1-4 DISTANCE        (A) : NULL  ; NULL
REMARK   3    H-BOND OR METAL COORDINATION    (A) : NULL  ; NULL
REMARK   3
REMARK   3   PLANE RESTRAINT                  (A) : 0.013 ; 0.020
REMARK   3   CHIRAL-CENTER RESTRAINT       (A**3) : NULL  ; NULL
REMARK   3
REMARK   3   NON-BONDED CONTACT RESTRAINTS.
REMARK   3    SINGLE TORSION                  (A) : NULL  ; NULL
REMARK   3    MULTIPLE TORSION                (A) : NULL  ; NULL
REMARK   3    H-BOND (X...Y)                  (A) : NULL  ; NULL
REMARK   3    H-BOND (X-H...Y)                (A) : NULL  ; NULL
REMARK   3
REMARK   3   CONFORMATIONAL TORSION ANGLE RESTRAINTS.
REMARK   3    SPECIFIED                 (DEGREES) : NULL  ; NULL
REMARK   3    PLANAR                    (DEGREES) : NULL  ; NULL
REMARK   3    STAGGERED                 (DEGREES) : NULL  ; NULL
REMARK   3    TRANSVERSE                (DEGREES) : NULL  ; NULL
REMARK   3
REMARK   3  ISOTROPIC THERMAL FACTOR RESTRAINTS.    RMS    SIGMA
REMARK   3   MAIN-CHAIN BOND              (A**2) : NULL  ; NULL
REMARK   3   MAIN-CHAIN ANGLE             (A**2) : NULL  ; NULL
REMARK   3   SIDE-CHAIN BOND              (A**2) : NULL  ; NULL
REMARK   3   SIDE-CHAIN ANGLE             (A**2) : NULL  ; NULL
REMARK   3
REMARK   3  OTHER REFINEMENT REMARKS:
REMARK   3  TNT BY TRONRUD, TEN EYCK, MATTHEWS ALSO WAS USED.
REMARK   3      BOND ANGLES                                3.4(3.00)
REMARK   4
REMARK   4 1DIN COMPLIES WITH FORMAT V. 2.0, 16-FEB-1996
REMARK   6
REMARK   6 THERE IS MICROHETEROGENEITY AT RESIDUE 123.  ONE OF THE
REMARK   6 RESIDUES IS CYSTEINE AND THE OTHER IS OXIDIZED CYSTEINE
REMARK   6 WHICH IS PRESENTED AS RESIDUE CSD.  ONLY CSD IS LISTED ON
REMARK   6 THE SEQRES RECORDS BELOW; BOTH CYS AND CSD ARE LISTED ON
REMARK   6 SEQADV RECORDS.  COORDINATES ARE PRESENTED FOR CYS AND
REMARK   6 CSD.
REMARK 200
REMARK 200 EXPERIMENTAL DETAILS
REMARK 200  EXPERIMENT TYPE                : X-RAY DIFFRACTION
REMARK 200  DATE OF DATA COLLECTION        : 1987
REMARK 200  TEMPERATURE           (KELVIN) : NULL
REMARK 200  PH                             : NULL
REMARK 200  NUMBER OF CRYSTALS USED        : NULL
REMARK 200
REMARK 200  SYNCHROTRON              (Y/N) : N
REMARK 200  RADIATION SOURCE               : NULL
REMARK 200  BEAMLINE                       : NULL
REMARK 200  X-RAY GENERATOR MODEL          : NULL
REMARK 200  MONOCHROMATIC OR LAUE    (M/L) : M
REMARK 200  WAVELENGTH OR RANGE        (A) : 1.5418
REMARK 200  MONOCHROMATOR                  : NULL
REMARK 200  OPTICS                         : NULL
REMARK 200
REMARK 200  DETECTOR TYPE                  : NICOLET
REMARK 200  DETECTOR MANUFACTURER          : NULL
REMARK 200  INTENSITY-INTEGRATION SOFTWARE : XENGEN
REMARK 200  DATA SCALING SOFTWARE          : NULL
REMARK 200
REMARK 200  NUMBER OF UNIQUE REFLECTIONS   : 29488
REMARK 200  RESOLUTION RANGE HIGH      (A) : NULL
REMARK 200  RESOLUTION RANGE LOW       (A) : NULL
REMARK 200  REJECTION CRITERIA  (SIGMA(I)) : NULL
REMARK 200
REMARK 200 OVERALL.
REMARK 200  COMPLETENESS FOR RANGE     (%) : 95.
REMARK 200  DATA REDUNDANCY                : 6.
REMARK 200  R MERGE                    (I) : 0.057
REMARK 200  R SYM                      (I) : NULL
REMARK 200  <I/SIGMA(I)> FOR THE DATA SET  : NULL
REMARK 200
REMARK 200 IN THE HIGHEST RESOLUTION SHELL.
REMARK 200  HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : NULL
REMARK 200  HIGHEST RESOLUTION SHELL, RANGE LOW  (A) : NULL
REMARK 200  COMPLETENESS FOR SHELL     (%) : NULL
REMARK 200  DATA REDUNDANCY IN SHELL       : NULL
REMARK 200  R MERGE FOR SHELL          (I) : NULL
REMARK 200  R SYM FOR SHELL            (I) : NULL
REMARK 200  <I/SIGMA(I)> FOR SHELL         : NULL
REMARK 200
REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: NULL
REMARK 200 SOFTWARE USED: NULL
REMARK 200 STARTING MODEL: NULL
REMARK 200
REMARK 200 REMARK: NULL
REMARK 280
REMARK 280 CRYSTAL
REMARK 280 SOLVENT CONTENT, VS   (%): NULL
REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): NULL
REMARK 280
REMARK 280 CRYSTALLIZATION CONDITIONS: NULL
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   1/2-X,-Y,1/2+Z
REMARK 290       3555   -X,1/2+Y,1/2-Z
REMARK 290       4555   1/2+X,1/2-Y,-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       24.44988
REMARK 290   SMTRY2   2  0.000000 -1.000000  0.000000        0.00000
REMARK 290   SMTRY3   2  0.000000  0.000000  1.000000       39.12057
REMARK 290   SMTRY1   3 -1.000000  0.000000  0.000000        0.00000
REMARK 290   SMTRY2   3  0.000000  1.000000  0.000000       35.72449
REMARK 290   SMTRY3   3  0.000000  0.000000 -1.000000       39.12057
REMARK 290   SMTRY1   4  1.000000  0.000000  0.000000       24.44988
REMARK 290   SMTRY2   4  0.000000 -1.000000  0.000000       35.72449
REMARK 290   SMTRY3   4  0.000000  0.000000 -1.000000        0.00000
REMARK 290
REMARK 290 REMARK: NULL
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     SER   233    O
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.  SOME OF THESE MAY BE ATOMS
REMARK 500 LOCATED ON SPECIAL POSITIONS IN THE CELL.
REMARK 500
REMARK 500 DISTANCE CUTOFF: 2.2 ANGSTROMS
REMARK 500
REMARK 500  ATM1  RES C  SSEQI   ATM2  RES C  SSEQI  SSYMOP   DISTANCE
REMARK 500   O    HOH     509     O    HOH     481     2665     1.63
REMARK 999
REMARK 999 SEQUENCE
REMARK 999 1DIN       SWS     P11453     234 -   236 NOT IN ATOMS LIST
REMARK 999
REMARK 999   THE ORIGINAL SEQUENCE WAS INCORRECT AT POSITION 79.  THE
REMARK 999   CORRECT SEQUENCE IS REPORTED IN CHEAH, E., AUSTIN, C.,
REMARK 999   ASHLEY, G., OLLIS, D., PROTEIN ENGINEERING, VOL 6,
REMARK 999   PAGES 575-583 (1993).
DBREF  1DIN      1   233  SWS    P11453   CLCD_PSEPU       1    233
SEQADV 1DIN CSD    123  SWS  P11453    CYS   123 CONFLICT
SEQADV 1DIN CYS    123  SWS  P11453    CYS   123 MICROHETEROGENEITY
SEQADV 1DIN ASN    154  SWS  P11453    LYS   154 CONFLICT
SEQADV 1DIN THR    224  SWS  P11453    ARG   224 CONFLICT
SEQRES   1    236  MET LEU THR GLU GLY ILE SER ILE GLN SER TYR ASP GLY
SEQRES   2    236  HIS THR PHE GLY ALA LEU VAL GLY SER PRO ALA LYS ALA
SEQRES   3    236  PRO ALA PRO VAL ILE VAL ILE ALA GLN GLU ILE PHE GLY
SEQRES   4    236  VAL ASN ALA PHE MET ARG GLU THR VAL SER TRP LEU VAL
SEQRES   5    236  ASP GLN GLY TYR ALA ALA VAL CYS PRO ASP LEU TYR ALA
SEQRES   6    236  ARG GLN ALA PRO GLY THR ALA LEU ASP PRO GLN ASP GLU
SEQRES   7    236  ARG GLN ARG GLU GLN ALA TYR LYS LEU TRP GLN ALA PHE
SEQRES   8    236  ASP MET GLU ALA GLY VAL GLY ASP LEU GLU ALA ALA ILE
SEQRES   9    236  ARG TYR ALA ARG HIS GLN PRO TYR SER ASN GLY LYS VAL
SEQRES  10    236  GLY LEU VAL GLY TYR CSD LEU GLY GLY ALA LEU ALA PHE
SEQRES  11    236  LEU VAL ALA ALA LYS GLY TYR VAL ASP ARG ALA VAL GLY
SEQRES  12    236  TYR TYR GLY VAL GLY LEU GLU LYS GLN LEU ASN LYS VAL
SEQRES  13    236  PRO GLU VAL LYS HIS PRO ALA LEU PHE HIS MET GLY GLY
SEQRES  14    236  GLN ASP HIS PHE VAL PRO ALA PRO SER ARG GLN LEU ILE
SEQRES  15    236  THR GLU GLY PHE GLY ALA ASN PRO LEU LEU GLN VAL HIS
SEQRES  16    236  TRP TYR GLU GLU ALA GLY HIS SER PHE ALA ARG THR SER
SEQRES  17    236  SER SER GLY TYR VAL ALA SER ALA ALA ALA LEU ALA ASN
SEQRES  18    236  GLU ARG THR LEU ASP PHE LEU ALA PRO LEU GLN SER LYS
SEQRES  19    236  LYS PRO
MODRES 1DIN CSD    123  CYS  MODIFIED CYSTEINE
HET    CSD    123       8
HETNAM     CSD 3-SULFINOALANINE
HETSYN     CSD S-CYSTEINESULFINIC ACID; S-SULFINOCYSTEINE
FORMUL   1  CSD    C3 H7 N1 O4 S1
FORMUL   2  HOH   *279(H2 O1)
HELIX    1   2 LEU     63  ALA     68  5                                   6
HELIX    2   3 GLU     78  GLN     89  1                                  12
HELIX    3   4 MET     93  HIS    109  1                                  17
HELIX    4   5 GLY    125  LYS    135  1                                  11
HELIX    5   6 LEU    149  GLU    158  5                                  10
HELIX    6   7 ALA    176  ALA    188  1                                  13
HELIX    7   8 ALA    214  LEU    231  1                                  18
SHEET    1   A 7 ALA    18  GLY    21  0
SHEET    2   A 7 ALA    57  PRO    61 -1  N  CYS    60   O  LEU    19
SHEET    3   A 7 VAL    30  ALA    34  1  N  ILE    31   O  ALA    57
SHEET    4   A 7 VAL   117  GLY   121  1  N  GLY   118   O  VAL    30
SHEET    5   A 7 ARG   140  TYR   144  1  N  ARG   140   O  LEU   119
SHEET    6   A 7 ALA   163  GLY   168  1  N  LEU   164   O  ALA   141
SHEET    7   A 7 LEU   192  TYR   197  1  N  GLN   193   O  ALA   163
LINK         N   CSD   123                 C   TYR   122
LINK         C   CSD   123                 N   LEU   124
CISPEP   1 ALA     26    PRO     27          0        -1.55
CRYST1   48.900   71.450   78.240  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      0.020450  0.000000  0.000000        0.00000
SCALE2      0.000000  0.013996  0.000000        0.00000
SCALE3      0.000000  0.000000  0.012781        0.00000