data_15515 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR STRUCTURAL STUDIES OF THE ANTIBIOTIC LIPOPEPTIDE DAPTOMYCIN IN DHPC MICELLES ; _BMRB_accession_number 15515 _BMRB_flat_file_name bmr15515.str _Entry_type new _Submission_date 2007-10-09 _Accession_date 2007-10-09 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Scott W. R.P. . 2 Baek S. . . 3 Jung D. . . 4 Hancock R. E.W. . 5 Straus S. K. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 60 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-06-26 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_citations _Saveframe_category entry_citation _Citation_title 'NMR structural studies of the antibiotic lipopeptide daptomycin in DHPC micelles' _Citation_status published _Citation_type journal _PubMed_ID 17945184 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Scott W. R.P. . 2 Baek S. . . 3 Jung D. . . 4 Hancock R. E. . 5 Straus S. K. . stop_ _Journal_abbreviation 'Biochim. Biophys. Acta' _Journal_volume 1768 _Journal_issue 12 _Journal_ASTM VIER _Journal_ISSN 0005-2736 _Page_first 3116 _Page_last 3126 _Year 2007 save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'daptomycin in DHPC' loop_ _Mol_system_component_name _Mol_label DAPTOMYCIN $DAPTOMYCIN 'CALCIUM ION' $CA stop_ _System_physical_state native _System_oligomer_state ? _System_paramagnetic no save_ ######################## # Monomeric polymers # ######################## save_DAPTOMYCIN _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common DAPTOMYCIN _Molecular_mass 1639.711 _Mol_thiol_state 'not present' loop_ _Biological_function antibiotic stop_ ############################## # Polymer residue sequence # ############################## _Residue_count 14 _Mol_residue_sequence XWXDTGXDXDGXXX loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 0 DKA 2 1 TRP 3 2 DSG 4 3 ASP 5 4 THR 6 5 GLY 7 6 ORN 8 7 ASP 9 8 DAL 10 9 ASP 11 10 GLY 12 11 DSN 13 12 MEG 14 13 KYN stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_DKA _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 'DECANOIC ACID' _PDB_code DKA _Standard_residue_derivative . _Mol_empirical_formula 'C10 H20 O2' _Molecular_mass 172.265 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 20:34:44 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C N 0 . ? O1 O1 O N 0 . ? C2 C2 C N 0 . ? C3 C3 C N 0 . ? C4 C4 C N 0 . ? C5 C5 C N 0 . ? C6 C6 C N 0 . ? C7 C7 C N 0 . ? C8 C8 C N 0 . ? C9 C9 C N 0 . ? C10 C10 C N 0 . ? O2 O2 O N 0 . ? H21 H21 H N 0 . ? H22 H22 H N 0 . ? H31 H31 H N 0 . ? H32 H32 H N 0 . ? H41 H41 H N 0 . ? H42 H42 H N 0 . ? H51 H51 H N 0 . ? H52 H52 H N 0 . ? H61 H61 H N 0 . ? H62 H62 H N 0 . ? H71 H71 H N 0 . ? H72 H72 H N 0 . ? H81 H81 H N 0 . ? H82 H82 H N 0 . ? H91 H91 H N 0 . ? H92 H92 H N 0 . ? H101 H101 H N 0 . ? H102 H102 H N 0 . ? H103 H103 H N 0 . ? HO2 HO2 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 DOUB C1 O1 C1 O1 SING C1 C2 C1 C2 SING C1 O2 C1 O2 SING C2 C3 C2 C3 SING C2 H21 C2 H21 SING C2 H22 C2 H22 SING C3 C4 C3 C4 SING C3 H31 C3 H31 SING C3 H32 C3 H32 SING C4 C5 C4 C5 SING C4 H41 C4 H41 SING C4 H42 C4 H42 SING C5 C6 C5 C6 SING C5 H51 C5 H51 SING C5 H52 C5 H52 SING C6 C7 C6 C7 SING C6 H61 C6 H61 SING C6 H62 C6 H62 SING C7 C8 C7 C8 SING C7 H71 C7 H71 SING C7 H72 C7 H72 SING C8 C9 C8 C9 SING C8 H81 C8 H81 SING C8 H82 C8 H82 SING C9 C10 C9 C10 SING C9 H91 C9 H91 SING C9 H92 C9 H92 SING C10 H101 C10 H101 SING C10 H102 C10 H102 SING C10 H103 C10 H103 SING O2 HO2 O2 HO2 stop_ save_ save_chem_comp_DSG _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-ASPARAGINE _PDB_code DSG _Standard_residue_derivative . _Mol_empirical_formula 'C4 H8 N2 O3' _Molecular_mass 132.118 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 20:48:34 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 R 0 . ? C C C N 0 . ? O O O N 0 . ? CB CB C N 0 . ? CG CG C N 0 . ? OD1 OD1 O N 0 . ? ND2 ND2 N N 0 . ? OXT OXT O N 0 . ? H H H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HD21 HD21 H N 0 . ? HD22 HD22 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 H N H SING N HN2 N HN2 SING CA C CA C SING CA CB CA CB SING CA HA CA HA DOUB C O C O SING C OXT C OXT SING CB CG CB CG SING CB HB1 CB HB1 SING CB HB2 CB HB2 DOUB CG OD1 CG OD1 SING CG ND2 CG ND2 SING ND2 HD21 ND2 HD21 SING ND2 HD22 ND2 HD22 SING OXT HXT OXT HXT stop_ save_ save_chem_comp_ORN _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common ORNITHINE _PDB_code ORN _Standard_residue_derivative . _Mol_empirical_formula 'C5 H14 N2 O2' _Molecular_mass 134.177 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Aug 21 00:51:13 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N N 1 . ? CA CA C S 0 . ? CB CB C N 0 . ? CG CG C N 0 . ? CD CD C N 0 . ? NE NE N N 1 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? HN1 HN1 H N 0 . ? HN2 HN2 H N 0 . ? HN3 HN3 H N 0 . ? HA HA H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HG1 HG1 H N 0 . ? HG2 HG2 H N 0 . ? HD1 HD1 H N 0 . ? HD2 HD2 H N 0 . ? HNE1 HNE1 H N 0 . ? HNE2 HNE2 H N 0 . ? HNE3 HNE3 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 HN1 N HN1 SING N HN2 N HN2 SING N HN3 N HN3 SING CA CB CA CB SING CA C CA C SING CA HA CA HA SING CB CG CB CG SING CB HB1 CB HB1 SING CB HB2 CB HB2 SING CG CD CG CD SING CG HG1 CG HG1 SING CG HG2 CG HG2 SING CD NE CD NE SING CD HD1 CD HD1 SING CD HD2 CD HD2 SING NE HNE1 NE HNE1 SING NE HNE2 NE HNE2 SING NE HNE3 NE HNE3 DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT stop_ save_ save_chem_comp_DAL _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-ALANINE _PDB_code DAL _Standard_residue_derivative . _Mol_empirical_formula 'C3 H7 N O2' _Molecular_mass 89.093 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 20:18:27 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 R 0 . ? CB CB C N 0 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? H H H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HB3 HB3 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 H N H SING N HN2 N HN2 SING CA CB CA CB SING CA C CA C SING CA HA CA HA SING CB HB1 CB HB1 SING CB HB2 CB HB2 SING CB HB3 CB HB3 DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT stop_ save_ save_chem_comp_DSN _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-SERINE _PDB_code DSN _Standard_residue_derivative . _Mol_empirical_formula 'C3 H7 N O3' _Molecular_mass 105.093 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 20:48:42 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 R 0 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? CB CB C N 0 . ? OG OG O N 0 . ? H H H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HXT HXT H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HOG HOG 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 H N H SING N HN2 N HN2 SING CA C CA C SING CA CB CA CB SING CA HA CA HA DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT SING CB OG CB OG SING CB HB1 CB HB1 SING CB HB2 CB HB2 SING OG HOG OG HOG stop_ save_ save_chem_comp_MEG _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common '(2S,3R)-3-METHYL-GLUTAMIC ACID' _PDB_code MEG _Standard_residue_derivative . _Mol_empirical_formula 'C6 H11 N O4' _Molecular_mass 161.156 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 23:39:13 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 . ? CB CB C S 0 . ? CG CG C N 0 . ? CD CD C N 0 . ? OE1 OE1 O N 0 . ? OE2 OE2 O N 0 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? C1 C1 C N 0 . ? H H H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HB HB H N 0 . ? HG1 HG1 H N 0 . ? HG2 HG2 H N 0 . ? HXT HXT H N 0 . ? H11 H11 H N 0 . ? H12 H12 H N 0 . ? H13 H13 H N 0 . ? HO1 HO1 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 H N H SING N HN2 N HN2 SING CA CB CA CB SING CA C CA C SING CA HA CA HA SING CB CG CB CG SING CB C1 CB C1 SING CB HB CB HB SING CG CD CG CD SING CG HG1 CG HG1 SING CG HG2 CG HG2 DOUB CD OE1 CD OE1 SING CD OE2 CD OE2 DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT SING C1 H11 C1 H11 SING C1 H12 C1 H12 SING C1 H13 C1 H13 SING HO1 OE2 HO1 OE2 stop_ save_ save_chem_comp_KYN _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common KYNURENINE _PDB_code KYN _Standard_residue_derivative . _Mol_empirical_formula 'C10 H12 N2 O3' _Molecular_mass 208.214 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 23:08:43 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 R 0 . ? CB CB C N 0 . ? CG CG C N 0 . ? CD1 CD1 C N 0 . ? CE1 CE1 C N 0 . ? CZ CZ C N 0 . ? CE2 CE2 C N 0 . ? CD2 CD2 C N 0 . ? C C C N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? C1 C1 C N 0 . ? O2 O2 O N 0 . ? N1 N1 N N 0 . ? H H H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HD1 HD1 H N 0 . ? HE1 HE1 H N 0 . ? HZ HZ H N 0 . ? HE2 HE2 H N 0 . ? HXT HXT H N 0 . ? H11 H11 H N 0 . ? H12 H12 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 H N H SING N HN2 N HN2 SING CA CB CA CB SING CA C CA C SING CA HA CA HA SING CB C1 CB C1 SING CB HB1 CB HB1 SING CB HB2 CB HB2 DOUB CG CD1 CG CD1 SING CG CD2 CG CD2 SING CG N1 CG N1 SING CD1 CE1 CD1 CE1 SING CD1 HD1 CD1 HD1 DOUB CE1 CZ CE1 CZ SING CE1 HE1 CE1 HE1 SING CZ CE2 CZ CE2 SING CZ HZ CZ HZ DOUB CE2 CD2 CE2 CD2 SING CE2 HE2 CE2 HE2 SING CD2 C1 CD2 C1 DOUB C O C O SING C OXT C OXT SING OXT HXT OXT HXT DOUB C1 O2 C1 O2 SING N1 H11 N1 H11 SING N1 H12 N1 H12 stop_ save_ ############# # Ligands # ############# save_CA _Saveframe_category ligand _Mol_type non-polymer _Name_common "CA (CALCIUM ION)" _PDB_code CA _Mol_empirical_formula Ca _Molecular_mass 40.078 _Mol_charge 2 _Mol_paramagnetic . _Mol_aromatic no _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 19:28:44 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons CA CA CA N 2 . ? stop_ _Mol_thiol_state . save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bonds _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single covalent DAPTOMYCIN 5 THR OG DAPTOMYCIN 14 KYN C stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $DAPTOMYCIN 'Streptomyces roseosporus' 67294 Bacteria . Streptomyces roseosporus 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 $DAPTOMYCIN 'purified from the natural source' . . . . ? 'STREPTOMYCES ROSEOSPORUS, FERMENTATION END PRODUCT' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '2.0MM DAPTOMYCIN, 100MM KCL, 100MM DHPC-d40, 0.2MM EDTA, 5MM CACL2' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $DAPTOMYCIN 2.0 mM 'natural abundance' $CA 5.0 mM 'natural abundance' KCL 100 mM 'natural abundance' DHPC-d40 100 mM . EDTA 0.2 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 2.0 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task 'chemical shift assignment' 'structure solution' stop_ save_ save_GROMOS _Saveframe_category software _Name GROMOS _Version GROMOS96 loop_ _Vendor _Address _Electronic_address 'van Gunsteren and Berendsen' . . stop_ loop_ _Task refinement stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer VARIAN _Model UNITY _Field_strength 500 save_ ############################# # NMR applied experiments # ############################# save_2D_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NOESY' _Sample_label $sample_1 save_ save_2D_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D TOCSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.7 . pH pressure 1 . atm temperature 318 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference 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 0.00 internal direct ? ? ? 1.000000000 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 loop_ _Software_label $TOPSPIN stop_ loop_ _Experiment_label '2D NOESY' '2D TOCSY' 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 DAPTOMYCIN 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 2 TRP H H 8.13 0.01 1 2 1 2 TRP HA H 4.69 0.01 1 3 1 2 TRP HB2 H 3.21 0.01 2 4 1 2 TRP HB3 H 3.11 0.01 2 5 1 2 TRP HD1 H 7.40 0.01 1 6 1 2 TRP HE1 H 10.20 0.01 1 7 1 2 TRP HE3 H 7.46 0.01 1 8 1 2 TRP HZ2 H 7.19 0.01 4 9 1 2 TRP HZ3 H 7.36 0.01 4 10 2 3 DSG H H 8.07 0.01 1 11 2 3 DSG HA H 4.65 0.01 1 12 2 3 DSG HB2 H 2.57 0.01 2 13 2 3 DSG HD21 H 7.43 0.01 2 14 2 3 DSG HD22 H 6.75 0.01 2 15 3 4 ASP H H 8.09 0.01 1 16 3 4 ASP HA H 4.37 0.01 1 17 3 4 ASP HB2 H 2.54 0.01 2 18 3 4 ASP HB3 H 2.65 0.01 2 19 4 5 THR H H 8.08 0.01 1 20 4 5 THR HA H 4.52 0.01 1 21 4 5 THR HB H 5.39 0.01 1 22 4 5 THR HG2 H 1.10 0.01 1 23 5 6 GLY H H 8.30 0.01 1 24 5 6 GLY HA2 H 3.99 0.01 2 25 5 6 GLY HA3 H 3.89 0.02 2 26 6 7 ORN H H 8.09 0.01 1 27 6 7 ORN HA H 4.29 0.01 1 28 6 7 ORN HB2 H 1.79 0.01 2 29 6 7 ORN HB3 H 1.88 0.02 2 30 6 7 ORN HG H 1.71 0.01 1 31 7 8 ASP H H 8.31 0.01 1 32 7 8 ASP HA H 4.53 0.01 1 33 7 8 ASP HB2 H 2.58 0.01 2 34 7 8 ASP HB3 H 2.66 0.01 2 35 8 9 DAL H H 8.26 0.01 1 36 8 9 DAL HA H 4.30 0.01 1 37 8 9 DAL HB H 1.39 0.01 1 38 9 10 ASP H H 7.85 0.01 1 39 9 10 ASP HA H 4.58 0.03 9 40 9 10 ASP HB2 H 2.77 0.01 2 41 9 10 ASP HB3 H 2.66 0.01 2 42 10 11 GLY H H 8.23 0.01 1 43 10 11 GLY HA2 H 4.05 0.01 2 44 10 11 GLY HA3 H 3.94 0.01 2 45 11 12 DSN H H 8.38 0.01 1 46 11 12 DSN HA H 4.74 0.01 1 47 11 12 DSN HB2 H 3.88 0.01 2 48 12 13 MEG H H 8.03 0.01 1 49 12 13 MEG HA H 4.50 0.01 1 50 12 13 MEG HB2 H 2.44 0.01 2 51 12 13 MEG HG11 H 2.34 0.01 1 52 12 13 MEG HG12 H 2.34 0.01 1 53 12 13 MEG HG13 H 2.34 0.01 1 54 12 13 MEG HG2 H 0.88 0.01 1 55 13 14 KYN H H 8.44 0.02 1 56 13 14 KYN HA H 4.87 0.01 1 57 13 14 KYN HB2 H 3.45 0.01 2 58 13 14 KYN HB3 H 3.36 0.01 2 59 13 14 KYN HE1 H 7.62 0.01 4 60 13 14 KYN HE3 H 6.56 0.01 4 stop_ loop_ _Atom_shift_assign_ID_ambiguity 8 9 '59,60' stop_ save_