data_15284 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone 1H Chemical Shift Assignments for N-Me-Leu8 ; _BMRB_accession_number 15284 _BMRB_flat_file_name bmr15284.str _Entry_type new _Submission_date 2007-06-06 _Accession_date 2007-06-06 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Sabo Jennifer K. . 2 Harris Karen S. . 3 Coley Andrew M. . 4 Karas John A. . 5 Casey Joanne L. . 6 Tan 'Yen Yee' . . 7 Norton Raymond S. . 8 Hughes Andrew B. . 9 Scanlon Denis . . 10 Foley Michael . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 111 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2009-04-17 update BMRB 'complete entry citation' 2009-02-06 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 15282 N-Me-Phe5 15285 N-Me-Lys11 15287 N-Me-Phe12 15291 N-Me-Gly13 15292 N-Me-Ser14 15293 N-Me-Leu8/N-Me-Ser14 15294 N-Me-Val1/N-Me-Leu8/N-Me-Ser14 stop_ save_ ############################# # Citation for this entry # ############################# save_N-Me-Leu8_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Rapid optimization of a peptide inhibitor of malaria parasite invasion by comprehensive N-methyl scanning.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 19164290 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Harris Karen S. . 2 Casey Joanne L. . 3 Coley Andrew M. . 4 Karas John A. . 5 Sabo Jennifer K. . 6 Tan 'Yen Yee' . . 7 Dolezal Olan . . 8 Norton Raymond S. . 9 Hughes Andrew B. . 10 Scanlon Denis . . 11 Foley Michael . . stop_ _Journal_abbreviation 'J. Biol. Chem.' _Journal_name_full 'The Journal of biological chemistry' _Journal_volume 284 _Journal_issue 14 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 9361 _Page_last 9371 _Year 2009 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name N-Me-Leu8 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label N-Me-Leu8 $N-Me-Leu8 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'Methylation of the backbone amide for Leu8' save_ ######################## # Monomeric polymers # ######################## save_N-Me-Leu8 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common N-Me-Leu8 _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 20 _Mol_residue_sequence VFAEFLPXFSKFGSRMHILK loop_ _Residue_seq_code _Residue_label 1 VAL 2 PHE 3 ALA 4 GLU 5 PHE 6 LEU 7 PRO 8 2ML 9 PHE 10 SER 11 LYS 12 PHE 13 GLY 14 SER 15 ARG 16 MET 17 HIS 18 ILE 19 LEU 20 LYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_2ML _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 2-METHYLLEUCINE _BMRB_code . _PDB_code 2ML _Standard_residue_derivative . _Molecular_mass 145.199 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Jun 18 15:58:21 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N N 0 . ? CA CA C S 0 . ? CB1 CB1 C N 0 . ? CB2 CB2 C N 0 . ? CG CG C N 0 . ? CD1 CD1 C N 0 . ? CD2 CD2 C N 0 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? HN2 HN2 H N 0 . ? H H H N 0 . ? HB11 HB11 H N 0 . ? HB12 HB12 H N 0 . ? HB21 HB21 H N 0 . ? HB22 HB22 H N 0 . ? HB23 HB23 H N 0 . ? HG HG H N 0 . ? HD11 HD11 H N 0 . ? HD12 HD12 H N 0 . ? HD13 HD13 H N 0 . ? HD21 HD21 H N 0 . ? HD22 HD22 H N 0 . ? HD23 HD23 H N 0 . ? HXT HXT H N 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N CA N CA SING N HN2 N HN2 SING N H N H SING CA CB1 CA CB1 SING CA CB2 CA CB2 SING CA C CA C SING CB1 CG CB1 CG SING CB1 HB11 CB1 HB11 SING CB1 HB12 CB1 HB12 SING CB2 HB21 CB2 HB21 SING CB2 HB22 CB2 HB22 SING CB2 HB23 CB2 HB23 SING CG CD1 CG CD1 SING CG CD2 CG CD2 SING CG HG CG HG SING CD1 HD11 CD1 HD11 SING CD1 HD12 CD1 HD12 SING CD1 HD13 CD1 HD13 SING CD2 HD21 CD2 HD21 SING CD2 HD22 CD2 HD22 SING CD2 HD23 CD2 HD23 DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $N-Me-Leu8 . . . . . . stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name _Details $N-Me-Leu8 'chemical synthesis' . . . . . 'solid-phase peptide synthesis' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '95 % H2O / 5 % 2H2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $N-Me-Leu8 1.7 mM 'natural abundance' H2O 95 % . D2O 5 % . stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 1.3 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 600 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 278 0.1 K pH 4.6 0.2 pH pressure 1 . atm stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS H 1 'methyl protons' ppm 0.0 internal direct . . . 1.0 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $TOPSPIN stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D DQF-COSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name N-Me-Leu8 _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 1 VAL HA H 3.75 0.02 1 2 1 1 VAL HB H 2.17 0.02 1 3 1 1 VAL HG1 H 0.99 0.02 1 4 2 2 PHE H H 8.81 0.02 1 5 2 2 PHE HA H 4.65 0.02 1 6 2 2 PHE HB3 H 3.08 0.02 1 7 2 2 PHE HD1 H 7.26 0.02 1 8 2 2 PHE HE1 H 7.36 0.02 1 9 3 3 ALA H H 8.39 0.02 1 10 3 3 ALA HA H 4.22 0.02 1 11 3 3 ALA HB H 1.26 0.02 1 12 4 4 GLU H H 8.26 0.02 1 13 4 4 GLU HA H 4.12 0.02 1 14 4 4 GLU HB2 H 1.84 0.02 2 15 4 4 GLU HB3 H 1.90 0.02 2 16 4 4 GLU HG2 H 2.13 0.02 2 17 4 4 GLU HG3 H 2.20 0.02 2 18 5 5 PHE H H 8.43 0.02 1 19 5 5 PHE HA H 4.62 0.02 1 20 5 5 PHE HB2 H 3.03 0.02 2 21 5 5 PHE HB3 H 3.06 0.02 2 22 5 5 PHE HD1 H 7.23 0.02 1 23 5 5 PHE HE1 H 7.33 0.02 1 24 6 6 LEU H H 8.16 0.02 1 25 6 6 LEU HA H 4.59 0.02 1 26 6 6 LEU HB3 H 1.49 0.02 1 27 6 6 LEU HD2 H 0.88 0.02 1 28 7 7 PRO HA H 4.57 0.02 1 29 7 7 PRO HB2 H 1.56 0.02 2 30 7 7 PRO HB3 H 2.22 0.02 2 31 7 7 PRO HD2 H 3.59 0.02 2 32 7 7 PRO HD3 H 3.71 0.02 2 33 7 7 PRO HG3 H 2.00 0.02 1 34 8 8 2ML H H 2.81 0.02 1 35 8 8 2ML HA H 4.56 0.02 1 36 8 8 2ML HB3 H 1.50 0.02 1 37 8 8 2ML HD11 H 0.79 0.02 1 38 8 8 2ML HD12 H 0.79 0.02 1 39 8 8 2ML HD13 H 0.79 0.02 1 40 8 8 2ML HD21 H 0.89 0.02 1 41 8 8 2ML HD22 H 0.89 0.02 1 42 8 8 2ML HD23 H 0.89 0.02 1 43 8 8 2ML HG H 1.40 0.02 1 44 9 9 PHE H H 8.04 0.02 1 45 9 9 PHE HA H 4.68 0.02 1 46 9 9 PHE HB2 H 2.94 0.02 2 47 9 9 PHE HB3 H 3.17 0.02 2 48 9 9 PHE HD1 H 7.24 0.02 1 49 9 9 PHE HE1 H 7.35 0.02 1 50 10 10 SER H H 8.48 0.02 1 51 10 10 SER HA H 4.41 0.02 1 52 10 10 SER HB2 H 3.79 0.02 2 53 10 10 SER HB3 H 3.88 0.02 2 54 11 11 LYS H H 8.48 0.02 1 55 11 11 LYS HA H 4.19 0.02 1 56 11 11 LYS HB3 H 1.62 0.02 1 57 11 11 LYS HD3 H 1.59 0.02 1 58 11 11 LYS HE3 H 2.90 0.02 1 59 11 11 LYS HG3 H 1.20 0.02 1 60 11 11 LYS HZ H 7.6 0.02 1 61 12 12 PHE H H 8.28 0.02 1 62 12 12 PHE HA H 4.63 0.02 1 63 12 12 PHE HB2 H 2.97 0.02 2 64 12 12 PHE HB3 H 3.21 0.02 2 65 12 12 PHE HD1 H 7.25 0.02 1 66 12 12 PHE HE1 H 7.36 0.02 1 67 13 13 GLY H H 8.34 0.02 1 68 13 13 GLY HA2 H 3.87 0.02 2 69 13 13 GLY HA3 H 3.98 0.02 2 70 14 14 SER H H 8.31 0.02 1 71 14 14 SER HA H 4.42 0.02 1 72 14 14 SER HB2 H 3.86 0.02 2 73 14 14 SER HB3 H 3.90 0.02 2 74 15 15 ARG H H 8.53 0.02 1 75 15 15 ARG HA H 4.32 0.02 1 76 15 15 ARG HB2 H 1.75 0.02 2 77 15 15 ARG HB3 H 1.87 0.02 2 78 15 15 ARG HD3 H 3.15 0.02 1 79 15 15 ARG HE H 7.22 0.02 1 80 15 15 ARG HG3 H 1.62 0.02 1 81 16 16 MET H H 8.34 0.02 1 82 16 16 MET HA H 4.38 0.02 1 83 16 16 MET HB3 H 1.94 0.02 1 84 16 16 MET HG2 H 2.44 0.02 2 85 16 16 MET HG3 H 2.52 0.02 2 86 17 17 HIS H H 8.63 0.02 1 87 17 17 HIS HA H 4.70 0.02 1 88 17 17 HIS HB2 H 3.11 0.02 2 89 17 17 HIS HB3 H 3.21 0.02 2 90 17 17 HIS HD2 H 7.24 0.02 1 91 17 17 HIS HE1 H 8.58 0.02 1 92 18 18 ILE H H 8.34 0.02 1 93 18 18 ILE HA H 4.11 0.02 1 94 18 18 ILE HB H 1.81 0.02 1 95 18 18 ILE HD1 H 0.84 0.02 1 96 18 18 ILE HG12 H 1.15 0.02 1 97 18 18 ILE HG13 H 1.44 0.02 1 98 18 18 ILE HG2 H 0.87 0.02 1 99 19 19 LEU H H 8.55 0.02 1 100 19 19 LEU HA H 4.37 0.02 1 101 19 19 LEU HB3 H 1.62 0.02 1 102 19 19 LEU HD1 H 0.87 0.02 1 103 19 19 LEU HD2 H 0.93 0.02 1 104 20 20 LYS H H 7.98 0.02 1 105 20 20 LYS HA H 4.14 0.02 1 106 20 20 LYS HB2 H 1.71 0.02 2 107 20 20 LYS HB3 H 1.79 0.02 2 108 20 20 LYS HD3 H 1.66 0.02 1 109 20 20 LYS HE3 H 2.97 0.02 1 110 20 20 LYS HG3 H 1.37 0.02 1 111 20 20 LYS HZ H 7.59 0.02 1 stop_ save_