*HEADER PROTEIN BINDING 17-APR-08 SMS20022 *TITLE 1H CHEMICAL SHIFT ASSIGNMENTS FOR METASTIN ANALOG, S5A *COMPND MOL_ID: 1; *COMPND 2 MOLECULE: KISSPEPTIN-10; *COMPND 3 CHAIN: A; *COMPND 4 FRAGMENT: UNP RESIDUES 112-121; *COMPND 5 SYNONYM: METASTASIS-SUPPRESSOR KISS-1; *COMPND 6 ENGINEERED: YES; *COMPND 7 OTHER_DETAILS: GPCR LIGAND, METASTIN ANALOG *SOURCE MOL_ID: 1; *SOURCE 2 SYNTHETIC: YES; *SOURCE 3 ORGANISM_SCIENTIFIC: HOMO SAPIENS; *SOURCE 4 ORGANISM_COMMON: HUMAN; *SOURCE 5 ORGANISM_TAXID: 9606; *SOURCE 6 OTHER_DETAILS: SOLID PHASE PEPTIDE SYNTHESIS USING FMOC CHEMISTRY *KEYWDS PROTEIN BINDING *EXPDTA SOLUTION NMR *NUMMDL 1 *AUTHOR J.I.KIM !s5a {dihedral} restraints dihedral reset assign (resid 1 and name c ) (resid 2 and name n ) (resid 2 and name ca ) (resid 2 and name c ) 1 -120.0 40.0 2 assign (resid 2 and name c ) (resid 3 and name n ) (resid 3 and name ca ) (resid 3 and name c ) 1 -120.0 40.0 2 assign (resid 3 and name c ) (resid 4 and name n ) (resid 4 and name ca ) (resid 4 and name c ) 1 -120.0 40.0 2 assign (resid 4 and name c ) (resid 5 and name n ) (resid 5 and name ca ) (resid 5 and name c ) 1 -120.0 40.0 2 assign (resid 5 and name c ) (resid 6 and name n ) (resid 6 and name ca ) (resid 6 and name c ) 1 -120.0 40.0 2 assign (resid 6 and name c ) (resid 7 and name n ) (resid 7 and name ca ) (resid 7 and name c ) 1 -120.0 40.0 2 assign (resid 7 and name c ) (resid 8 and name n ) (resid 8 and name ca ) (resid 8 and name c ) 1 -120.0 40.0 2 assign (resid 8 and name c ) (resid 9 and name n ) (resid 9 and name ca ) (resid 9 and name c ) 1 -120.0 40.0 2 assign (resid 9 and name c ) (resid 10 and name n ) (resid 10 and name ca ) (resid 10 and name c ) 1 -120.0 40.0 2 end ! ANSIG v3.3 XPLOR distance restraints file ! No distance corrections applied. ! Trivial distances output. ! residue 1 Tyr , NOEs forward in sequence assi (resi 1 and name HD# ) (resi 2 and name HN ) 4.00 2.20 3.40 assi (resi 1 and name HB# ) (resi 3 and name HD1 ) 4.00 2.20 3.00 assi (resi 1 and name HA ) (resi 2 and name HN ) 2.50 0.70 0.20 assi (resi 1 and name HB# ) (resi 2 and name HN ) 3.00 1.20 0.50 assi (resi 1 and name HB# ) (resi 2 and name HB# ) 3.00 1.20 1.50 ! residue 2 Asn , NOEs forward in sequence assi (resi 2 and name HA ) (resi 3 and name HN ) 2.50 0.70 1.20 assi (resi 2 and name HB# ) (resi 3 and name HN ) 3.00 1.20 1.50 assi (resi 2 and name HB# ) (resi 3 and name HB# ) 3.00 1.20 1.50 assi (resi 2 and name HB# ) (resi 4 and name HN ) 3.00 1.20 1.50 assi (resi 2 and name HD2#) (resi 5 and name HB# ) 4.00 2.20 3.00 assi (resi 2 and name HB# ) (resi 5 and name HB# ) 4.00 2.20 4.00 assi (resi 2 and name HA ) (resi 3 and name HD1 ) 3.00 1.20 1.50 assi (resi 2 and name HN ) (resi 5 and name HB# ) 4.00 2.20 2.00 ! residue 3 Trp , NOEs forward in sequence assi (resi 3 and name HA ) (resi 4 and name HN ) 2.50 0.70 0.80 assi (resi 3 and name HN ) (resi 4 and name HB# ) 4.00 2.20 2.00 assi (resi 3 and name HD1 ) (resi 4 and name HN ) 4.00 2.20 2.00 assi (resi 3 and name HN ) (resi 4 and name HN ) 2.50 0.70 0.20 assi (resi 3 and name HN ) (resi 4 and name HA ) 4.00 2.20 1.00 assi (resi 3 and name HB# ) (resi 4 and name HN ) 3.00 1.20 1.50 assi (resi 3 and name HE3 ) (resi 4 and name HN ) 4.00 2.20 2.00 assi (resi 3 and name HE3 ) (resi 6 and name HB# ) 4.00 2.20 2.00 assi (resi 3 and name HB# ) (resi 6 and name HB# ) 4.00 2.20 3.00 assi (resi 3 and name HE3 ) (resi 4 and name HA ) 4.00 2.20 2.00 ! residue 4 Asn , NOEs forward in sequence assi (resi 4 and name HA ) (resi 5 and name HN ) 2.50 0.70 0.80 assi (resi 4 and name HN ) (resi 5 and name HN ) 2.50 0.70 0.20 assi (resi 4 and name HB# ) (resi 5 and name HN ) 3.00 1.20 1.50 assi (resi 4 and name HN ) (resi 5 and name HA ) 4.00 2.20 3.00 assi (resi 4 and name HN ) (resi 5 and name HB# ) 4.00 2.20 2.00 assi (resi 4 and name HD2#) (resi 5 and name HN ) 4.00 2.20 2.00 ! residue 5 Ala , NOEs forward in sequence assi (resi 5 and name HA ) (resi 6 and name HN ) 2.50 0.70 0.20 assi (resi 5 and name HB# ) (resi 6 and name HN ) 3.00 1.20 1.50 assi (resi 5 and name HB# ) (resi 6 and name HD# ) 4.00 2.20 4.00 assi (resi 5 and name HN ) (resi 7 and name HN ) 4.00 2.20 1.00 assi (resi 5 and name HN ) (resi 9 and name HN ) 3.00 1.20 1.50 assi (resi 5 and name HB# ) (resi 7 and name HN ) 4.00 2.20 3.00 ! residue 6 Phe , NOEs forward in sequence assi (resi 6 and name HA ) (resi 7 and name HN ) 3.00 1.20 0.50 assi (resi 6 and name HA ) (resi 9 and name HN ) 4.00 2.20 1.00 assi (resi 6 and name HB# ) (resi 7 and name HN ) 3.00 1.20 1.50 assi (resi 6 and name HB# ) (resi 8 and name HN ) 4.00 2.20 2.00 assi (resi 6 and name HB# ) (resi 10 and name HB# ) 4.00 2.20 3.00 assi (resi 6 and name HN ) (resi 9 and name HN ) 4.00 2.20 1.60 assi (resi 6 and name HD# ) (resi 8 and name HD# ) 4.00 2.20 5.80 assi (resi 6 and name HN ) (resi 7 and name HN ) 3.00 1.20 0.50 ! residue 7 Gly , NOEs forward in sequence assi (resi 7 and name HA# ) (resi 8 and name HN ) 3.00 1.20 1.50 assi (resi 7 and name HN ) (resi 8 and name HN ) 2.50 0.70 0.20 assi (resi 7 and name HN ) (resi 8 and name HB# ) 4.00 2.20 3.00 assi (resi 7 and name HN ) (resi 9 and name HN ) 4.00 2.20 1.00 ! residue 8 Leu , NOEs forward in sequence assi (resi 8 and name HN ) (resi 9 and name HN ) 2.50 0.70 0.20 assi (resi 8 and name HG ) (resi 9 and name HN ) 3.00 1.20 0.50 assi (resi 8 and name HD# ) (resi 9 and name HN ) 4.00 2.20 2.00 assi (resi 8 and name HG ) (resi 10 and name HN ) 4.00 2.20 1.00 assi (resi 8 and name HB# ) (resi 10 and name HN ) 4.00 2.20 2.00 assi (resi 8 and name HD# ) (resi 10 and name HD# ) 4.00 2.20 6.80 ! residue 9 Arg , NOEs forward in sequence assi (resi 9 and name HA ) (resi 10 and name HN ) 2.50 0.70 1.20 assi (resi 9 and name HA ) (resi 10 and name HE# ) 4.00 2.20 4.40 assi (resi 9 and name HN ) (resi 10 and name HN ) 3.00 1.20 0.50 assi (resi 9 and name HB# ) (resi 10 and name HN ) 3.00 1.20 1.50 assi (resi 9 and name HB# ) (resi 10 and name HD# ) 4.00 2.20 4.40 assi (resi 9 and name HG# ) (resi 10 and name HN ) 4.00 2.20 2.00 assi (resi 9 and name HG# ) (resi 10 and name HD# ) 4.00 2.20 4.40 ! ANSIG v3.3 XPLOR distance restraints file ! No distance corrections applied. ! Trivial distances output. ! residue 1 Tyr , intraresidue NOEs assi (resi 1 and name HA ) (resi 1 and name HE# ) 4.00 2.20 3.40 assi (resi 1 and name HA ) (resi 1 and name HD# ) 3.00 1.20 1.50 assi (resi 1 and name HA ) (resi 1 and name HB# ) 3.00 1.20 1.50 assi (resi 1 and name HB# ) (resi 1 and name HD# ) 3.00 1.20 2.50 assi (resi 1 and name HB# ) (resi 1 and name HE# ) 4.00 2.20 3.10 ! residue 2 Asn , intraresidue NOEs assi (resi 2 and name HN ) (resi 2 and name HA ) 3.00 1.20 0.50 assi (resi 2 and name HN ) (resi 2 and name HB# ) 3.00 1.20 1.10 assi (resi 2 and name HA ) (resi 2 and name HB# ) 3.00 1.20 1.10 assi (resi 2 and name HB# ) (resi 2 and name HD2#) 4.00 2.20 2.60 ! residue 3 Trp , intraresidue NOEs assi (resi 3 and name HN ) (resi 3 and name HA ) 3.00 1.20 0.50 assi (resi 3 and name HN ) (resi 3 and name HB# ) 3.00 1.20 1.10 assi (resi 3 and name HA ) (resi 3 and name HD1 ) 4.00 2.20 2.00 assi (resi 3 and name HA ) (resi 3 and name HE3 ) 3.00 1.20 2.50 assi (resi 3 and name HA ) (resi 3 and name HB# ) 3.00 1.20 1.10 assi (resi 3 and name HD1 ) (resi 3 and name HB# ) 3.00 1.20 2.10 assi (resi 3 and name HE3 ) (resi 3 and name HZ2 ) 4.00 2.20 2.00 assi (resi 3 and name HE3 ) (resi 3 and name HZ3 ) 2.50 0.70 1.20 assi (resi 3 and name HE3 ) (resi 3 and name HH2 ) 4.00 2.20 2.00 assi (resi 3 and name HE3 ) (resi 3 and name HB# ) 3.00 1.20 2.70 assi (resi 3 and name HZ2 ) (resi 3 and name HZ3 ) 3.00 1.20 1.50 assi (resi 3 and name HZ2 ) (resi 3 and name HH2 ) 2.50 0.70 1.20 assi (resi 3 and name HZ3 ) (resi 3 and name HH2 ) 4.00 2.20 1.00 ! residue 4 Asn , intraresidue NOEs assi (resi 4 and name HN ) (resi 4 and name HA ) 2.50 0.70 0.20 assi (resi 4 and name HN ) (resi 4 and name HB# ) 2.50 0.70 0.80 assi (resi 4 and name HA ) (resi 4 and name HB# ) 2.50 0.70 0.80 assi (resi 4 and name HB# ) (resi 4 and name HD2#) 4.00 2.20 2.60 assi (resi 4 and name HN ) (resi 4 and name HD2#) 4.00 2.20 4.40 ! residue 5 Ala , intraresidue NOEs assi (resi 5 and name HN ) (resi 5 and name HA ) 2.50 0.70 0.20 assi (resi 5 and name HN ) (resi 5 and name HB# ) 2.50 0.70 0.80 assi (resi 5 and name HA ) (resi 5 and name HB# ) 2.50 0.70 0.80 ! residue 6 Phe , intraresidue NOEs assi (resi 6 and name HN ) (resi 6 and name HA ) 2.50 0.70 0.20 assi (resi 6 and name HN ) (resi 6 and name HB# ) 3.00 1.20 1.50 assi (resi 6 and name HN ) (resi 6 and name HD# ) 4.00 2.20 3.40 assi (resi 6 and name HA ) (resi 6 and name HB# ) 3.00 1.20 1.50 assi (resi 6 and name HA ) (resi 6 and name HD# ) 3.00 1.20 2.50 assi (resi 6 and name HB# ) (resi 6 and name HD# ) 3.00 1.20 2.50 ! residue 7 Gly , intraresidue NOEs assi (resi 7 and name HN ) (resi 7 and name HA# ) 2.50 0.70 0.80 ! residue 8 Leu , intraresidue NOEs assi (resi 8 and name HN ) (resi 8 and name HA ) 2.50 0.70 0.20 assi (resi 8 and name HN ) (resi 8 and name HG1 ) 3.00 1.20 0.50 assi (resi 8 and name HN ) (resi 8 and name HB# ) 2.50 0.70 0.80 assi (resi 8 and name HN ) (resi 8 and name HD# ) 4.00 2.20 2.00 assi (resi 8 and name HA ) (resi 8 and name HG1 ) 3.00 1.20 0.50 assi (resi 8 and name HA ) (resi 8 and name HB# ) 3.00 1.20 1.10 assi (resi 8 and name HA ) (resi 8 and name HD# ) 3.00 1.20 2.20 assi (resi 8 and name HG1 ) (resi 8 and name HD# ) 3.00 1.20 1.10 assi (resi 8 and name HB# ) (resi 8 and name HD# ) 3.00 1.20 2.10 ! residue 9 Arg , intraresidue NOEs00 assi (resi 9 and name HN ) (resi 9 and name HA ) 2.50 0.70 0.20 assi (resi 9 and name HN ) (resi 9 and name HB# ) 2.50 0.70 0.80 assi (resi 9 and name HN ) (resi 9 and name HG# ) 3.00 1.20 1.50 assi (resi 9 and name HN ) (resi 9 and name HD# ) 4.00 2.20 3.00 assi (resi 9 and name HA ) (resi 9 and name HB# ) 2.50 0.70 0.80 assi (resi 9 and name HA ) (resi 9 and name HG# ) 3.00 1.20 1.10 assi (resi 9 and name HA ) (resi 9 and name HD# ) 4.00 2.20 2.00 assi (resi 9 and name HA ) (resi 9 and name HE ) 4.00 2.20 3.00 assi (resi 9 and name HE ) (resi 9 and name HB# ) 4.00 2.20 2.00 assi (resi 9 and name HE ) (resi 9 and name HG# ) 3.00 1.20 1.10 assi (resi 9 and name HE ) (resi 9 and name HD# ) 2.50 0.70 1.40 assi (resi 9 and name HB# ) (resi 9 and name HG# ) 2.50 0.70 1.40 assi (resi 9 and name HB# ) (resi 9 and name HD# ) 3.00 1.20 2.00 assi (resi 9 and name HG# ) (resi 9 and name HD# ) 2.50 0.70 1.40 ! residue 10 Phe , intraresidue NOEs assi (resi 10 and name HN ) (resi 10 and name HA ) 3.00 1.20 0.50 assi (resi 10 and name HN ) (resi 10 and name HB# ) 3.00 1.20 1.10 assi (resi 10 and name HN ) (resi 10 and name HD# ) 4.00 2.20 3.40 assi (resi 10 and name HN ) (resi 10 and name HE# ) 4.00 2.20 3.40 assi (resi 10 and name HA ) (resi 10 and name HB# ) 3.00 1.20 1.10 assi (resi 10 and name HA ) (resi 10 and name HE# ) 4.00 2.20 3.40 assi (resi 10 and name HA ) (resi 10 and name HD# ) 4.00 2.20 3.40 assi (resi 10 and name HB# ) (resi 10 and name HD# ) 4.00 2.20 3.00 assi (resi 10 and name HB# ) (resi 10 and name HE# ) 4.00 2.20 3.10 residue J(Hz) 2N 13.75 3W 13.93 4N 13.75 5A 14.04 6F 13.75 7G 13.64 8L 13.69 9R 13.77 10F 13.75 Entry H atom name Submitted Coord H atom name 1 H1 TYR 1 HT1 TYR 1 -0.133 5.554 1.952 2 H2 TYR 1 HT2 TYR 1 0.386 6.967 2.740 3 H3 TYR 1 HT3 TYR 1 -1.111 6.271 3.138 4 HA TYR 1 HA TYR 1 0.292 5.604 4.886 5 HB2 TYR 1 HB2 TYR 1 0.363 3.414 2.801 6 HB3 TYR 1 HB1 TYR 1 0.295 3.216 4.552 7 HD1 TYR 1 HD2 TYR 1 -1.736 4.619 5.683 8 HD2 TYR 1 HD1 TYR 1 -1.645 3.150 1.647 9 HE1 TYR 1 HE2 TYR 1 -4.214 4.694 5.601 10 HE2 TYR 1 HE1 TYR 1 -4.123 3.225 1.565 11 HH TYR 1 HH TYR 1 -5.985 3.723 2.658 12 H ASN 2 HN ASN 2 2.143 3.483 4.606 13 HA ASN 2 HA ASN 2 4.620 4.985 4.257 14 HB2 ASN 2 HB2 ASN 2 3.867 2.128 4.922 15 HB3 ASN 2 HB1 ASN 2 5.530 2.717 4.943 16 HD21 ASN 2 HD21 ASN 2 2.383 2.969 6.558 17 HD22 ASN 2 HD22 ASN 2 2.956 3.783 7.933 18 H TRP 3 HN TRP 3 4.539 1.674 3.171 19 HA TRP 3 HA TRP 3 4.537 2.372 0.306 20 HB2 TRP 3 HB2 TRP 3 6.939 2.066 1.971 21 HB3 TRP 3 HB1 TRP 3 6.950 1.033 0.541 22 HD1 TRP 3 HD1 TRP 3 6.898 4.693 1.605 23 HE1 TRP 3 HE1 TRP 3 7.467 6.161 -0.439 24 HE3 TRP 3 HE3 TRP 3 6.865 1.145 -2.065 25 HZ2 TRP 3 HZ2 TRP 3 7.856 5.866 -3.260 26 HZ3 TRP 3 HZ3 TRP 3 7.335 1.762 -4.418 27 HH2 TRP 3 HH2 TRP 3 7.829 4.116 -5.021 28 H ASN 4 HN ASN 4 3.337 0.446 2.460 29 HA ASN 4 HA ASN 4 3.778 -2.053 0.929 30 HB2 ASN 4 HB2 ASN 4 3.655 -3.238 2.996 31 HB3 ASN 4 HB1 ASN 4 4.661 -1.830 3.335 32 HD21 ASN 4 HD21 ASN 4 2.311 -3.561 4.780 33 HD22 ASN 4 HD22 ASN 4 1.474 -2.335 5.603 34 H ALA 5 HN ALA 5 1.706 0.186 0.706 35 HA ALA 5 HA ALA 5 -0.614 -1.551 0.442 36 HB1 ALA 5 HB1 ALA 5 -0.241 -0.554 2.892 37 HB2 ALA 5 HB2 ALA 5 -1.859 -0.697 2.205 38 HB3 ALA 5 HB3 ALA 5 -1.019 0.854 2.169 39 H PHE 6 HN PHE 6 0.498 -0.371 -1.679 40 HA PHE 6 HA PHE 6 -1.477 1.594 -2.505 41 HB2 PHE 6 HB2 PHE 6 0.807 2.487 -1.241 42 HB3 PHE 6 HB1 PHE 6 1.237 2.616 -2.947 43 HD1 PHE 6 HD2 PHE 6 -1.210 3.290 -4.302 44 HD2 PHE 6 HD1 PHE 6 0.187 4.599 -0.456 45 HE1 PHE 6 HE2 PHE 6 -2.592 5.340 -4.497 46 HE2 PHE 6 HE1 PHE 6 -1.195 6.650 -0.652 47 HZ PHE 6 HZ PHE 6 -2.585 7.020 -2.673 48 H GLY 7 HN GLY 7 1.841 1.003 -3.628 49 HA2 GLY 7 HA2 GLY 7 0.759 0.325 -6.298 50 HA3 GLY 7 HA1 GLY 7 2.451 0.654 -5.926 51 H LEU 8 HN LEU 8 1.526 -1.338 -3.517 52 HA LEU 8 HA LEU 8 2.438 -3.735 -4.994 53 HB2 LEU 8 HB2 LEU 8 2.451 -3.406 -2.005 54 HB3 LEU 8 HB1 LEU 8 3.524 -4.380 -3.008 55 HG LEU 8 HG LEU 8 3.479 -1.357 -2.814 56 HD11 LEU 8 HD11 LEU 8 5.739 -1.648 -1.915 57 HD12 LEU 8 HD12 LEU 8 5.618 -3.395 -2.123 58 HD13 LEU 8 HD13 LEU 8 4.590 -2.574 -0.949 59 HD21 LEU 8 HD21 LEU 8 5.703 -2.518 -4.273 60 HD22 LEU 8 HD22 LEU 8 4.579 -1.259 -4.783 61 HD23 LEU 8 HD23 LEU 8 4.169 -2.957 -5.024 62 H ARG 9 HN ARG 9 0.451 -3.005 -2.110 63 HA ARG 9 HA ARG 9 -1.094 -5.434 -2.424 64 HB2 ARG 9 HB2 ARG 9 -0.841 -3.139 -0.560 65 HB3 ARG 9 HB1 ARG 9 -2.403 -3.959 -0.566 66 HG2 ARG 9 HG2 ARG 9 -1.453 -6.030 0.059 67 HG3 ARG 9 HG1 ARG 9 0.173 -5.518 -0.394 68 HD2 ARG 9 HD2 ARG 9 0.535 -4.781 1.716 69 HD3 ARG 9 HD1 ARG 9 -0.861 -3.694 1.585 70 HE ARG 9 HE ARG 9 -2.074 -6.115 1.952 71 HH11 ARG 9 HH21 ARG 9 -2.161 -4.247 4.205 72 HH12 ARG 9 HH22 ARG 9 -1.295 -5.081 5.452 73 HH21 ARG 9 HH11 ARG 9 0.208 -7.323 3.275 74 HH22 ARG 9 HH12 ARG 9 0.046 -6.822 4.925 75 H PHE 10 HN PHE 10 -1.392 -2.119 -3.455 76 HA PHE 10 HA PHE 10 -4.196 -2.664 -4.378 77 HB2 PHE 10 HB2 PHE 10 -2.735 -0.244 -3.341 78 HB3 PHE 10 HB1 PHE 10 -4.146 -0.034 -4.380 79 HD1 PHE 10 HD1 PHE 10 -3.034 -1.941 -1.345 80 HD2 PHE 10 HD2 PHE 10 -6.278 -0.045 -3.425 81 HE1 PHE 10 HE1 PHE 10 -4.527 -2.378 0.586 82 HE2 PHE 10 HE2 PHE 10 -7.771 -0.481 -1.494 83 HZ PHE 10 HZ PHE 10 -6.896 -1.648 0.511