TITLE THE 1.2 ANGSTROM STRUCTURE OF G1 ALPHA CONOTOXIN COMPND MOL_ID: 1; COMPND 2 MOLECULE: GI ALPHA CONOTOXIN; COMPND 3 CHAIN: NULL; COMPND 4 ENGINEERED: YES SOURCE MOL_ID: 1; SOURCE 2 SYNTHETIC: YES; SOURCE 4 ORGANISM_SCIENTIFIC: CONUS GEOGRAPHUS KEYWDS VENOM, DISULPHIDE LOOP, CONOTOXIN, ACETYLCHOLINE RECEPTOR EXPDTA X-RAY DIFFRACTION AUTHOR L.W.GUDDAT,L.SHAN,J.L.MARTIN,A.B.EDMUNDSON,W.R.GRAY REVDAT 1 07-DEC-96 1NOT 0 JRNL AUTH L.W.GUDDAT,J.L.MARTIN,L.SHAN,A.B.EDMUNDSON, JRNL AUTH 2 W.R.GRAY JRNL TITL THE THREE-DIMENSIONAL STRUCTURE OF THE JRNL TITL 2 ALPHA-CONOTOXIN GI AT 1.2 ANGSTROMS RESOLUTION JRNL REF TO BE PUBLISHED JRNL REFN 0353 REMARK 1 REMARK 1 REFERENCE 1 REMARK 1 AUTH A.PARDI,A.GALDES,J.FLORANCE,D.MANICONTE REMARK 1 TITL SOLUTION STRUCTURES OF ALPHA-CONOTOXIN G1 REMARK 1 TITL 2 DETERMINED BY TWO-DIMENSIONAL NMR SPECTROSCOPY REMARK 1 REF BIOCHEMISTRY V. 28 5494 1989 REMARK 1 REFN ASTM BICHAW US ISSN 0006-2960 0033 REMARK 2 REMARK 2 RESOLUTION. 1.2 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : X-PLOR 3.10 REMARK 3 AUTHORS : BRUNGER REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 1.2 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 6.0 REMARK 3 DATA CUTOFF (SIGMA(F)) : 2.0 REMARK 3 DATA CUTOFF HIGH (ABS(F)) : NULL REMARK 3 DATA CUTOFF LOW (ABS(F)) : NULL REMARK 3 COMPLETENESS (WORKING+TEST) (%) : 95.8 REMARK 3 NUMBER OF REFLECTIONS : 2960 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 CROSS-VALIDATION METHOD : RFREE REMARK 3 FREE R VALUE TEST SET SELECTION : RANDOM REMARK 3 R VALUE (WORKING SET) : 0.178 REMARK 3 FREE R VALUE : 0.222 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 10.0 REMARK 3 FREE R VALUE TEST SET COUNT : 306 REMARK 3 ESTIMATED ERROR OF FREE R VALUE : NULL REMARK 3 REMARK 3 FIT IN THE HIGHEST RESOLUTION BIN. REMARK 3 TOTAL NUMBER OF BINS USED : NULL REMARK 3 BIN RESOLUTION RANGE HIGH (A) : 1.20 REMARK 3 BIN RESOLUTION RANGE LOW (A) : 1.25 REMARK 3 BIN COMPLETENESS (WORKING+TEST) (%) : 83.6 REMARK 3 REFLECTIONS IN BIN (WORKING SET) : 292 REMARK 3 BIN R VALUE (WORKING SET) : 0.302 REMARK 3 BIN FREE R VALUE : 0.351 REMARK 3 BIN FREE R VALUE TEST SET SIZE (%) : 8.95 REMARK 3 BIN FREE R VALUE TEST SET COUNT : 35 REMARK 3 ESTIMATED ERROR OF BIN FREE R VALUE : NULL REMARK 3 REMARK 3 NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT. REMARK 3 PROTEIN ATOMS : 97 REMARK 3 NUCLEIC ACID ATOMS : 0 REMARK 3 HETEROGEN ATOMS : 0 REMARK 3 SOLVENT ATOMS : 21 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : NULL REMARK 3 MEAN B VALUE (OVERALL, A**2) : 15.9 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) : 0.17 REMARK 3 ESD FROM SIGMAA (A) : NULL REMARK 3 LOW RESOLUTION CUTOFF (A) : 6.0 REMARK 3 REMARK 3 CROSS-VALIDATED ESTIMATED COORDINATE ERROR. REMARK 3 ESD FROM C-V LUZZATI PLOT (A) : 0.23 REMARK 3 ESD FROM C-V SIGMAA (A) : NULL REMARK 3 REMARK 3 RMS DEVIATIONS FROM IDEAL VALUES. REMARK 3 BOND LENGTHS (A) : 0.007 REMARK 3 BOND ANGLES (DEGREES) : 1.72 REMARK 3 DIHEDRAL ANGLES (DEGREES) : 26.11 REMARK 3 IMPROPER ANGLES (DEGREES) : 1.41 REMARK 3 REMARK 3 ISOTROPIC THERMAL MODEL : NULL REMARK 3 REMARK 3 ISOTROPIC THERMAL FACTOR RESTRAINTS. RMS SIGMA REMARK 3 MAIN-CHAIN BOND (A**2) : NULL ; 1.50 REMARK 3 MAIN-CHAIN ANGLE (A**2) : NULL ; 2.00 REMARK 3 SIDE-CHAIN BOND (A**2) : NULL ; 2.00 REMARK 3 SIDE-CHAIN ANGLE (A**2) : NULL ; 2.50 REMARK 3 REMARK 3 NCS MODEL : NULL REMARK 3 REMARK 3 NCS RESTRAINTS. RMS SIGMA/WEIGHT REMARK 3 GROUP 1 POSITIONAL (A) : NULL ; NULL REMARK 3 GROUP 1 B-FACTOR (A**2) : NULL ; NULL REMARK 3 REMARK 3 PARAMETER FILE 1 : NULL REMARK 3 PARAMETER FILE 2 : NULL REMARK 3 TOPOLOGY FILE 1 : NULL REMARK 3 TOPOLOGY FILE 2 : NULL REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: NULL REMARK 4 REMARK 4 1NOT COMPLIES WITH FORMAT V. 2.1, 25-OCT-1996 REMARK 6 REMARK 6 THE CARBOXYL TERMINUS IS N-AMIDATED. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 15-MAR-1995 REMARK 200 TEMPERATURE (KELVIN) : 287 REMARK 200 PH : 5.2 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : N REMARK 200 RADIATION SOURCE : RIGAKU RU200 REMARK 200 BEAMLINE : NULL REMARK 200 X-RAY GENERATOR MODEL : RU 200 REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.54182 REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : RAXIS IIC REMARK 200 DETECTOR MANUFACTURER : RIGAKU REMARK 200 INTENSITY-INTEGRATION SOFTWARE : PROCESS REMARK 200 DATA SCALING SOFTWARE : PROCESS REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 3597 REMARK 200 RESOLUTION RANGE HIGH (A) : 1.10 REMARK 200 RESOLUTION RANGE LOW (A) : 22.0 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : NULL REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 84.2 REMARK 200 DATA REDUNDANCY : 7.6 REMARK 200 R MERGE (I) : 0.0718 REMARK 200 R SYM (I) : NULL REMARK 200 <I/SIGMA(I)> FOR THE DATA SET : 13.64 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.10 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 1.20 REMARK 200 COMPLETENESS FOR SHELL (%) : 54.90 REMARK 200 DATA REDUNDANCY IN SHELL : 6.80 REMARK 200 R MERGE FOR SHELL (I) : 0.335 REMARK 200 R SYM FOR SHELL (I) : NULL REMARK 200 <I/SIGMA(I)> FOR SHELL : 4.23 REMARK 200 REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: DIRECT METHODS REMARK 200 SOFTWARE USED: SHAKE AND BAKE REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: REMARK 200 IF DIFFERENCE > 0.3*FHMEAN + 0.1FHSQ REMARK 200 REJECT PAIR IF DIFFERENCE > 3.0 TIMES ABOVE CRITERION REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 27. 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 1 21 1 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -X,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 0.00000 REMARK 290 SMTRY2 2 0.000000 1.000000 0.000000 7.30002 REMARK 290 SMTRY3 2 0.000000 0.000000 -1.000000 0.00000 REMARK 290 REMARK 290 REMARK: NULL REMARK 999 REMARK 999 SEQUENCE REMARK 999 1NOT SWS P01519 15 - 15 NOT IN ATOMS LIST DBREF 1NOT 1 14 SWS P01519 CXA1_CONGE 1 14 SEQADV 1NOT NH2 14 SWS P01519 GLY 14 CONFLICT SEQRES 1 14 GLU CYS CYS ASN PRO ALA CYS GLY ARG HIS TYR SER CYS SEQRES 2 14 NH2 HET NH2 14 1 HETNAM NH2 AMINO GROUP FORMUL 1 NH2 H2 N1 FORMUL 2 HOH *21(H2 O1) HELIX 1 1 PRO 5 HIS 10 5 6 SSBOND 1 CYS 2 CYS 7 SSBOND 2 CYS 3 CYS 13 LINK N NH2 14 C CYS 13 CRYST1 14.900 14.600 22.600 90.00 100.29 90.00 P 1 21 1 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 0.067114 0.000000 0.012185 0.00000 SCALE2 0.000000 0.068493 0.000000 0.00000 SCALE3 0.000000 0.000000 0.044971 0.00000 ATOM 1 N GLU 1 -6.189 3.090 -1.547 1.00 29.06 N ATOM 2 CA GLU 1 -5.068 2.140 -1.800 1.00 25.34 C ATOM 3 C GLU 1 -5.386 1.202 -2.948 1.00 19.50 C ATOM 4 O GLU 1 -6.549 0.955 -3.257 1.00 21.67 O ATOM 5 CB GLU 1 -4.770 1.283 -0.562 1.00 27.67 C ATOM 6 CG GLU 1 -4.024 1.993 0.558 1.00 34.82 C ATOM 7 CD GLU 1 -3.325 1.036 1.524 1.00 40.81 C ATOM 8 OE1 GLU 1 -3.629 -0.183 1.542 1.00 37.57 O ATOM 9 OE2 GLU 1 -2.458 1.522 2.279 1.00 37.21 O ATOM 10 N CYS 2 -4.333 0.651 -3.533 1.00 10.17 N ATOM 11 CA CYS 2 -4.429 -0.298 -4.633 1.00 7.19 C ATOM 12 C CYS 2 -3.225 -1.195 -4.366 1.00 7.88 C ATOM 13 O CYS 2 -2.076 -0.837 -4.664 1.00 9.25 O ATOM 14 CB CYS 2 -4.289 0.422 -5.972 1.00 6.33 C ATOM 15 SG CYS 2 -5.022 -0.514 -7.342 1.00 8.75 S ATOM 16 N CYS 3 -3.498 -2.342 -3.758 1.00 6.75 N ATOM 17 CA CYS 3 -2.473 -3.289 -3.334 1.00 7.35 C ATOM 18 C CYS 3 -2.321 -4.528 -4.185 1.00 7.54 C ATOM 19 O CYS 3 -1.435 -5.340 -3.943 1.00 10.12 O ATOM 20 CB CYS 3 -2.772 -3.726 -1.904 1.00 7.25 C ATOM 21 SG CYS 3 -2.617 -2.387 -0.684 1.00 11.52 S ATOM 22 N ASN 4 -3.184 -4.692 -5.173 1.00 7.66 N ATOM 23 CA ASN 4 -3.114 -5.875 -6.021 1.00 6.97 C ATOM 24 C ASN 4 -2.082 -5.708 -7.113 1.00 6.94 C ATOM 25 O ASN 4 -1.861 -4.605 -7.597 1.00 6.94 O ATOM 26 CB ASN 4 -4.467 -6.124 -6.689 1.00 13.57 C ATOM 27 CG ASN 4 -5.634 -5.821 -5.778 1.00 18.92 C ATOM 28 OD1 ASN 4 -6.321 -4.792 -5.938 1.00 16.30 O ATOM 29 ND2 ASN 4 -5.856 -6.691 -4.798 1.00 15.61 N ATOM 30 N PRO 5 -1.432 -6.810 -7.527 1.00 7.27 N ATOM 31 CA PRO 5 -0.443 -6.700 -8.599 1.00 8.01 C ATOM 32 C PRO 5 -1.047 -6.044 -9.845 1.00 7.00 C ATOM 33 O PRO 5 -0.388 -5.255 -10.522 1.00 8.66 O ATOM 34 CB PRO 5 -0.096 -8.154 -8.874 1.00 8.95 C ATOM 35 CG PRO 5 -0.152 -8.756 -7.503 1.00 12.22 C ATOM 36 CD PRO 5 -1.395 -8.146 -6.903 1.00 8.70 C ATOM 37 N ALA 6 -2.323 -6.335 -10.119 1.00 6.44 N ATOM 38 CA ALA 6 -3.003 -5.778 -11.300 1.00 8.61 C ATOM 39 C ALA 6 -3.124 -4.258 -11.273 1.00 8.17 C ATOM 40 O ALA 6 -3.462 -3.636 -12.280 1.00 9.79 O ATOM 41 CB ALA 6 -4.383 -6.431 -11.490 1.00 7.32 C ATOM 42 N CYS 7 -2.877 -3.647 -10.122 1.00 7.11 N ATOM 43 CA CYS 7 -2.921 -2.195 -10.024 1.00 6.73 C ATOM 44 C CYS 7 -1.895 -1.566 -10.947 1.00 6.56 C ATOM 45 O CYS 7 -2.092 -0.448 -11.418 1.00 7.81 O ATOM 46 CB CYS 7 -2.603 -1.750 -8.608 1.00 9.01 C ATOM 47 SG CYS 7 -3.888 -2.197 -7.423 1.00 7.73 S ATOM 48 N GLY 8 -0.782 -2.262 -11.179 1.00 7.71 N ATOM 49 CA GLY 8 0.245 -1.742 -12.065 1.00 8.76 C ATOM 50 C GLY 8 0.708 -0.358 -11.668 1.00 9.91 C ATOM 51 O GLY 8 1.068 -0.118 -10.510 1.00 7.90 O ATOM 52 N ARG 9 0.627 0.583 -12.596 1.00 7.93 N ATOM 53 CA ARG 9 1.067 1.940 -12.315 1.00 7.92 C ATOM 54 C ARG 9 0.269 2.647 -11.226 1.00 8.21 C ATOM 55 O ARG 9 0.693 3.677 -10.711 1.00 9.28 O ATOM 56 CB ARG 9 1.072 2.783 -13.582 1.00 9.62 C ATOM 57 CG ARG 9 -0.298 3.134 -14.131 1.00 9.90 C ATOM 58 CD ARG 9 -0.094 4.081 -15.298 1.00 16.75 C ATOM 59 NE ARG 9 -1.323 4.552 -15.932 1.00 18.21 N ATOM 60 CZ ARG 9 -1.829 5.770 -15.768 1.00 14.96 C ATOM 61 NH1 ARG 9 -1.301 6.607 -14.884 1.00 14.61 N ATOM 62 NH2 ARG 9 -2.928 6.112 -16.416 1.00 22.37 N ATOM 63 N HIS 10 -0.883 2.094 -10.869 1.00 6.56 N ATOM 64 CA HIS 10 -1.723 2.694 -9.840 1.00 6.41 C ATOM 65 C HIS 10 -1.453 2.091 -8.477 1.00 5.41 C ATOM 66 O HIS 10 -2.133 2.415 -7.508 1.00 9.16 O ATOM 67 CB HIS 10 -3.207 2.526 -10.200 1.00 5.03 C ATOM 68 CG HIS 10 -3.559 3.119 -11.527 1.00 7.28 C ATOM 69 ND1 HIS 10 -3.598 4.477 -11.746 1.00 10.37 N ATOM 70 CD2 HIS 10 -3.802 2.536 -12.729 1.00 7.83 C ATOM 71 CE1 HIS 10 -3.843 4.712 -13.022 1.00 8.34 C ATOM 72 NE2 HIS 10 -3.969 3.551 -13.641 1.00 9.29 N ATOM 73 N TYR 11 -0.494 1.182 -8.409 1.00 6.33 N ATOM 74 CA TYR 11 -0.159 0.540 -7.143 1.00 6.60 C ATOM 75 C TYR 11 0.181 1.619 -6.109 1.00 6.66 C ATOM 76 O TYR 11 0.964 2.528 -6.377 1.00 8.78 O ATOM 77 CB TYR 11 1.027 -0.406 -7.329 1.00 6.84 C ATOM 78 CG TYR 11 1.455 -1.097 -6.042 1.00 9.80 C ATOM 79 CD1 TYR 11 0.904 -2.328 -5.654 1.00 16.46 C ATOM 80 CD2 TYR 11 2.415 -0.517 -5.210 1.00 9.97 C ATOM 81 CE1 TYR 11 1.298 -2.955 -4.473 1.00 11.18 C ATOM 82 CE2 TYR 11 2.815 -1.135 -4.033 1.00 15.52 C ATOM 83 CZ TYR 11 2.252 -2.346 -3.669 1.00 15.59 C ATOM 84 OH TYR 11 2.666 -2.958 -2.501 1.00 16.64 O ATOM 85 N SER 12 -0.457 1.538 -4.950 1.00 6.91 N ATOM 86 CA SER 12 -0.220 2.489 -3.871 1.00 9.13 C ATOM 87 C SER 12 -0.718 1.704 -2.677 1.00 10.01 C ATOM 88 O SER 12 -1.922 1.568 -2.474 1.00 11.17 O ATOM 89 CB SER 12 -1.040 3.759 -4.069 1.00 14.36 C ATOM 90 OG SER 12 -0.828 4.666 -2.999 1.00 16.91 O ATOM 91 N CYS 13 0.216 1.190 -1.892 1.00 11.57 N ATOM 92 CA CYS 13 -0.136 0.335 -0.785 1.00 8.32 C ATOM 93 C CYS 13 0.717 0.587 0.463 1.00 10.88 C ATOM 94 O CYS 13 1.951 0.466 0.373 1.00 12.41 O ATOM 95 CB CYS 13 0.041 -1.092 -1.292 1.00 10.69 C ATOM 96 SG CYS 13 -0.645 -2.394 -0.252 1.00 12.20 S HETATM 97 N NH2 14 0.102 0.945 1.575 1.00 13.69 N TER 98 NH2 14 HETATM 99 O HOH 14 -3.078 6.891 -2.983 1.00 35.65 O HETATM 100 O HOH 15 -2.894 4.700 -1.079 1.00 35.04 O HETATM 101 O HOH 16 -3.916 1.293 4.646 1.00 36.09 O HETATM 102 O HOH 17 -2.307 6.117 -19.184 1.00 44.73 O HETATM 103 O HOH 18 -0.025 -5.984 -13.389 1.00 48.15 O HETATM 104 O HOH 19 -4.348 -4.553 -14.731 1.00 20.88 O HETATM 105 O HOH 20 -2.846 8.846 -16.616 1.00 29.05 O HETATM 106 O HOH 21 5.343 -2.428 -0.454 1.00 47.20 O HETATM 107 O HOH 22 1.244 -6.344 -4.903 1.00 28.04 O HETATM 108 O HOH 23 -4.654 -9.814 -4.371 1.00 28.99 O HETATM 109 O HOH 24 -2.018 3.005 -18.550 1.00 35.75 O HETATM 110 O HOH 25 -3.837 -8.720 -9.314 1.00 7.86 O HETATM 111 O HOH 26 -4.105 4.117 -7.013 1.00 11.37 O HETATM 112 O HOH 27 0.509 6.181 -12.418 1.00 16.59 O HETATM 113 O HOH 28 2.450 3.331 -8.543 1.00 23.20 O HETATM 114 O HOH 29 2.840 4.655 -5.893 1.00 30.45 O HETATM 115 O HOH 30 1.789 5.807 -3.480 1.00 25.23 O HETATM 116 O HOH 31 0.135 -0.226 -15.277 1.00 19.06 O HETATM 117 O HOH 32 -6.277 -3.107 -3.296 1.00 28.80 O HETATM 118 O HOH 33 2.780 2.242 -2.212 1.00 20.57 O HETATM 119 O HOH 34 -4.324 -0.926 -13.401 1.00 18.98 O CONECT 15 14 47 CONECT 21 20 96 CONECT 47 15 46 CONECT 93 92 94 97 CONECT 96 21 95 CONECT 97 93 MASTER 183 0 1 1 0 0 0 6 118 1 6 2 END