data_27873 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of an alpha sheet hairpin peptide ; _BMRB_accession_number 27873 _BMRB_flat_file_name bmr27873.str _Entry_type original _Submission_date 2019-04-08 _Accession_date 2019-04-08 _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 Shea Dylan . . 2 Hsu Cheng-Chieh . . 3 Bi Timothy M. . 4 Paranjapye Natasha . . 5 Childers Matthew C. . 6 Cochran Joshua . . 7 Tomberlin Colson P. . 8 Wang Libo . . 9 Paris Daniel . . 10 Zonderman Jeffrey . . 11 Varani Gabriele . . 12 Link Christopher D. . 13 Mullan Mike . . 14 Daggett Valerie . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 coupling_constants 1 homonucl_NOEs 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 149 "13C chemical shifts" 75 "coupling constants" 6 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-05-09 original BMRB . stop_ _Original_release_date 2019-04-08 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; alpha-Sheet secondary structure in amyloid beta-peptide drives aggregation and toxicity in Alzheimer's disease ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 31004062 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shea Dylan . . 2 Hsu Cheng-Chieh C. . 3 Bi Timothy M. . 4 Paranjapye Natasha . . 5 Childers 'Matthew Carter' C. . 6 Cochran Joshua . . 7 Tomberlin Colson P. . 8 Wang Libo . . 9 Paris Daniel . . 10 Zonderman Jeffrey . . 11 Varani Gabriele . . 12 Link Christopher D. . 13 Mullan Mike . . 14 Daggett Valerie . . stop_ _Journal_abbreviation 'Proc. Natl. Acad. Sci. U.S.A.' _Journal_name_full 'Proceedings of the National Academy of Sciences of the United States of America' _Journal_volume 116 _Journal_issue 18 _Journal_ISSN 1091-6490 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8895 _Page_last 8900 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name AP407 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label AP407 $AP407 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'Inhibitor of amyloid aggregation' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_AP407 _Saveframe_category monomeric_polymer _Mol_type polymer _Name_common AP407 _Molecular_mass . _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function 'Inhibitor of amyloid aggregation' stop_ _Details ; This is a heterochiral polypeptide containing both L- and D-amino acids. In the one letter code, upper case letters refer to L-amino acids and lower case letters refer to D-amino acids. The N-terminus is acetylated and C-terminus is amidated. ; ############################## # Polymer residue sequence # ############################## _Residue_count 25 _Mol_residue_sequence ; XRGEXNXCXMNEYSGWXMXL XMGRX ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 0 ACE 2 1 ARG 3 2 GLY 4 3 GLU 5 4 MED 6 5 ASN 7 6 DLE 8 7 CYS 9 8 DTR 10 9 MET 11 10 ASN 12 11 GLU 13 12 TYR 14 13 SER 15 14 GLY 16 15 TRP 17 16 DCY 18 17 MET 19 18 DSG 20 19 LEU 21 20 DLY 22 21 MET 23 22 GLY 24 23 ARG 25 24 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ACE _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'ACETYL GROUP' _BMRB_code ACE _PDB_code ACE _Standard_residue_derivative . _Molecular_mass 44.053 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? O O O . 0 . ? CH3 CH3 C . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 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 C O ? ? SING C CH3 ? ? SING C H ? ? SING CH3 H1 ? ? SING CH3 H2 ? ? SING CH3 H3 ? ? stop_ save_ save_chem_comp_MED _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-METHIONINE _BMRB_code MED _PDB_code MED _Standard_residue_derivative . _Molecular_mass 149.211 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? SD SD S . 0 . ? CE CE C . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HE1 HE1 H . 0 . ? HE2 HE2 H . 0 . ? HE3 HE3 H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG SD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING SD CE ? ? SING CE HE1 ? ? SING CE HE2 ? ? SING CE HE3 ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DLE _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-LEUCINE _BMRB_code DLE _PDB_code DLE _Standard_residue_derivative . _Molecular_mass 131.173 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD1 CD1 C . 0 . ? CD2 CD2 C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG HG H . 0 . ? HD11 HD11 H . 0 . ? HD12 HD12 H . 0 . ? HD13 HD13 H . 0 . ? HD21 HD21 H . 0 . ? HD22 HD22 H . 0 . ? HD23 HD23 H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N H2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD1 ? ? SING CG CD2 ? ? SING CG HG ? ? SING CD1 HD11 ? ? SING CD1 HD12 ? ? SING CD1 HD13 ? ? SING CD2 HD21 ? ? SING CD2 HD22 ? ? SING CD2 HD23 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DTR _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-TRYPTOPHAN _BMRB_code DTR _PDB_code DTR _Standard_residue_derivative . _Molecular_mass 204.225 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD1 CD1 C . 0 . ? NE1 NE1 N . 0 . ? CE2 CE2 C . 0 . ? CZ2 CZ2 C . 0 . ? CH2 CH2 C . 0 . ? CZ3 CZ3 C . 0 . ? CE3 CE3 C . 0 . ? CD2 CD2 C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HD1 HD1 H . 0 . ? HE1 HE1 H . 0 . ? HZ2 HZ2 H . 0 . ? HH2 HH2 H . 0 . ? HZ3 HZ3 H . 0 . ? HE3 HE3 H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N HN2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? DOUB CG CD1 ? ? SING CG CD2 ? ? SING CD1 NE1 ? ? SING CD1 HD1 ? ? SING NE1 CE2 ? ? SING NE1 HE1 ? ? DOUB CE2 CZ2 ? ? SING CE2 CD2 ? ? SING CZ2 CH2 ? ? SING CZ2 HZ2 ? ? DOUB CH2 CZ3 ? ? SING CH2 HH2 ? ? SING CZ3 CE3 ? ? SING CZ3 HZ3 ? ? DOUB CE3 CD2 ? ? SING CE3 HE3 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DCY _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-CYSTEINE _BMRB_code DCY _PDB_code DCY _Standard_residue_derivative . _Molecular_mass 121.158 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? SG SG S . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG HG H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB SG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING SG HG ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DSG _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-ASPARAGINE _BMRB_code DSG _PDB_code DSG _Standard_residue_derivative . _Molecular_mass 132.118 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? OD1 OD1 O . 0 . ? ND2 ND2 N . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HD21 HD21 H . 0 . ? HD22 HD22 H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? DOUB CG OD1 ? ? SING CG ND2 ? ? SING ND2 HD21 ? ? SING ND2 HD22 ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DLY _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-LYSINE _BMRB_code DLY _PDB_code DLY _Standard_residue_derivative . _Molecular_mass 146.188 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? CE CE C . 0 . ? NZ NZ N . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD2 HD2 H . 0 . ? HD3 HD3 H . 0 . ? HE2 HE2 H . 0 . ? HE3 HE3 H . 0 . ? HZ1 HZ1 H . 0 . ? HZ2 HZ2 H . 0 . ? HXT HXT H . 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 ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING CD CE ? ? SING CD HD2 ? ? SING CD HD3 ? ? SING CE NZ ? ? SING CE HE2 ? ? SING CE HE3 ? ? SING NZ HZ1 ? ? SING NZ HZ2 ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 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 HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $AP407 . . . . . . 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 $AP407 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $AP407 800 uM 'natural abundance' 'potassium phosphate' 50 mM 'natural abundance' 'potassium chloride' 10 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _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 pH 5.8 . pH pressure 1 . atm temperature 273 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_reference_label_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 C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 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 _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $reference_label_1 _Mol_system_component_name AP407 _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 2 ARG H H 8.24 0.00 1 2 1 2 ARG HA H 4.16 0.01 1 3 1 2 ARG HB2 H 1.60 0.00 1 4 1 2 ARG HB3 H 1.71 0.00 1 5 1 2 ARG HG2 H 1.49 0.01 1 6 1 2 ARG HG3 H 1.51 0.01 1 7 1 2 ARG HD2 H 3.05 0.01 1 8 1 2 ARG HD3 H 3.05 0.01 1 9 1 2 ARG HE H 7.10 0.01 1 10 2 3 GLY H H 8.32 0.00 1 11 2 3 GLY HA2 H 3.74 0.02 1 12 2 3 GLY HA3 H 3.81 0.01 1 13 3 4 GLU H H 8.07 0.01 1 14 3 4 GLU HA H 4.03 0.02 1 15 3 4 GLU HB2 H 1.78 0.02 1 16 3 4 GLU HB3 H 1.88 0.02 1 17 3 4 GLU HG2 H 2.09 0.02 1 18 3 4 GLU HG3 H 2.09 0.02 1 19 4 5 MED H H 8.16 0.00 1 20 4 5 MED HA H 4.25 0.01 1 21 4 5 MED HB2 H 1.88 0.02 1 22 4 5 MED HB3 H 1.94 0.01 1 23 4 5 MED HG2 H 2.29 0.01 1 24 4 5 MED HG3 H 2.35 0.01 1 25 5 6 ASN H H 8.29 0.00 1 26 5 6 ASN HA H 4.67 0.01 1 27 5 6 ASN HB2 H 2.68 0.02 1 28 5 6 ASN HB3 H 2.74 0.01 1 29 5 6 ASN HD21 H 6.85 0.00 1 30 5 6 ASN HD22 H 7.41 0.00 1 31 6 7 DLE H H 8.16 0.00 1 32 6 7 DLE HA H 4.28 0.01 1 33 6 7 DLE HB2 H 1.56 0.01 1 34 6 7 DLE HB3 H 1.58 0.01 1 35 6 7 DLE HG H 1.52 0.01 1 36 6 7 DLE HD11 H 0.79 0.01 2 37 6 7 DLE HD12 H 0.79 0.01 2 38 6 7 DLE HD13 H 0.79 0.01 2 39 6 7 DLE HD21 H 0.83 0.01 2 40 6 7 DLE HD22 H 0.83 0.01 2 41 6 7 DLE HD23 H 0.83 0.01 2 42 7 8 CYS H H 8.60 0.01 1 43 7 8 CYS HA H 4.62 0.01 1 44 7 8 CYS HB2 H 2.80 0.02 1 45 7 8 CYS HB3 H 3.00 0.01 1 46 8 9 DTR H H 8.22 0.00 1 47 8 9 DTR HA H 4.50 0.02 1 48 8 9 DTR HB2 H 3.19 0.01 1 49 8 9 DTR HB3 H 3.19 0.01 1 50 8 9 DTR HD1 H 7.12 0.02 1 51 8 9 DTR HE1 H 10.13 0.00 1 52 8 9 DTR HE3 H 7.48 0.01 1 53 8 9 DTR HZ2 H 7.42 0.00 1 54 8 9 DTR HZ3 H 7.04 0.01 1 55 8 9 DTR HH2 H 7.12 0.02 1 56 9 10 MET H H 8.18 0.01 1 57 9 10 MET HA H 4.10 0.02 1 58 9 10 MET HB2 H 1.45 0.02 1 59 9 10 MET HB3 H 1.53 0.03 1 60 9 10 MET HG2 H 1.66 0.02 1 61 9 10 MET HG3 H 1.78 0.01 1 62 10 11 ASN H H 8.05 0.01 1 63 10 11 ASN HA H 4.51 0.01 1 64 10 11 ASN HB2 H 2.66 0.01 1 65 10 11 ASN HB3 H 2.73 0.01 1 66 10 11 ASN HD21 H 6.84 0.00 1 67 10 11 ASN HD22 H 7.44 0.00 1 68 11 12 GLU H H 8.26 0.01 1 69 11 12 GLU HA H 4.00 0.02 1 70 11 12 GLU HB2 H 1.76 0.02 1 71 11 12 GLU HB3 H 1.78 0.01 1 72 11 12 GLU HG2 H 1.98 0.03 1 73 11 12 GLU HG3 H 2.00 0.01 1 74 12 13 TYR H H 7.99 0.00 1 75 12 13 TYR HA H 4.49 0.02 1 76 12 13 TYR HB2 H 2.84 0.01 1 77 12 13 TYR HB3 H 3.04 0.02 1 78 12 13 TYR HD1 H 6.99 0.01 3 79 12 13 TYR HD2 H 6.99 0.01 3 80 12 13 TYR HE1 H 6.72 0.01 3 81 12 13 TYR HE2 H 6.72 0.01 3 82 13 14 SER H H 7.86 0.01 1 83 13 14 SER HA H 4.29 0.01 1 84 13 14 SER HB2 H 3.74 0.01 1 85 13 14 SER HB3 H 3.75 0.01 1 86 14 15 GLY H H 8.13 0.00 1 87 14 15 GLY HA2 H 3.76 0.01 1 88 14 15 GLY HA3 H 3.88 0.02 1 89 15 16 TRP H H 7.92 0.01 1 90 15 16 TRP HA H 4.59 0.02 1 91 15 16 TRP HB2 H 3.13 0.02 1 92 15 16 TRP HB3 H 3.19 0.01 1 93 15 16 TRP HD1 H 7.12 0.02 1 94 15 16 TRP HE1 H 10.04 0.00 1 95 15 16 TRP HE3 H 7.49 0.01 1 96 15 16 TRP HZ2 H 7.40 0.00 1 97 15 16 TRP HZ3 H 7.01 0.01 1 98 15 16 TRP HH2 H 7.13 0.02 1 99 16 17 DCY H H 8.00 0.01 1 100 16 17 DCY HA H 4.48 0.01 1 101 16 17 DCY HB2 H 2.66 0.01 1 102 16 17 DCY HB3 H 2.86 0.01 1 103 17 18 MET H H 8.39 0.00 1 104 17 18 MET HA H 4.32 0.01 1 105 17 18 MET HB2 H 1.93 0.01 1 106 17 18 MET HB3 H 1.99 0.01 1 107 17 18 MET HG2 H 2.44 0.01 1 108 17 18 MET HG3 H 2.50 0.01 1 109 18 19 DSG H H 8.35 0.01 1 110 18 19 DSG HA H 4.54 0.01 1 111 18 19 DSG HB2 H 2.63 0.03 1 112 18 19 DSG HB3 H 2.70 0.02 1 113 18 19 DSG HD21 H 6.80 0.01 1 114 18 19 DSG HD22 H 7.39 0.01 1 115 19 20 LEU H H 8.00 0.00 1 116 19 20 LEU HA H 4.22 0.02 1 117 19 20 LEU HB2 H 1.50 0.01 1 118 19 20 LEU HB3 H 1.54 0.01 1 119 19 20 LEU HG H 1.46 0.02 1 120 19 20 LEU HD1 H 0.75 0.02 2 121 19 20 LEU HD2 H 0.78 0.01 2 122 20 21 DLY H H 8.16 0.00 1 123 20 21 DLY HA H 4.17 0.01 1 124 20 21 DLY HB2 H 1.71 0.02 1 125 20 21 DLY HB3 H 1.74 0.01 1 126 20 21 DLY HG2 H 1.20 0.01 1 127 20 21 DLY HG3 H 1.28 0.02 1 128 20 21 DLY HD2 H 1.64 0.00 1 129 20 21 DLY HD3 H 1.65 0.00 1 130 20 21 DLY HE2 H 2.84 0.00 1 131 20 21 DLY HE3 H 2.84 0.00 1 132 21 22 MET H H 8.24 0.00 1 133 21 22 MET HA H 4.38 0.01 1 134 21 22 MET HB2 H 1.87 0.02 1 135 21 22 MET HB3 H 2.02 0.01 1 136 21 22 MET HG2 H 2.37 0.02 1 137 21 22 MET HG3 H 2.47 0.01 1 138 22 23 GLY H H 8.22 0.00 1 139 22 23 GLY HA2 H 3.81 0.01 1 140 22 23 GLY HA3 H 3.82 0.02 1 141 23 24 ARG H H 8.09 0.00 1 142 23 24 ARG HA H 4.19 0.02 1 143 23 24 ARG HB2 H 1.61 0.02 1 144 23 24 ARG HB3 H 1.75 0.01 1 145 23 24 ARG HG2 H 1.49 0.02 1 146 23 24 ARG HG3 H 1.51 0.01 1 147 23 24 ARG HD2 H 3.05 0.01 1 148 23 24 ARG HD3 H 3.05 0.01 1 149 23 24 ARG HE H 7.03 0.00 1 stop_ save_ save_assigned_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details ; There are two rows that could not be assigned to a specific atom: 12 TYR C 13 38.31 0.00 12 TYR C 13 42.09 0.00 ; loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $reference_label_1 _Mol_system_component_name AP407 _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 2 ARG CA C 56.51 0.00 1 2 1 2 ARG CB C 30.85 0.00 1 3 1 2 ARG CG C 27.05 0.00 1 4 1 2 ARG CD C 43.35 0.00 1 5 2 3 GLY CA C 45.31 0.00 1 6 3 4 GLU CA C 56.57 0.00 1 7 3 4 GLU CB C 30.29 0.00 1 8 3 4 GLU CG C 35.62 0.00 1 9 4 5 MED CA C 56.01 0.00 1 10 4 5 MED CB C 32.59 0.02 1 11 4 5 MED CG C 31.98 0.01 1 12 5 6 ASN CA C 53.31 0.00 1 13 5 6 ASN CB C 39.33 0.00 1 14 6 7 DLE CA C 55.80 0.00 1 15 6 7 DLE CB C 42.29 0.00 1 16 6 7 DLE CG C 27.06 0.00 1 17 6 7 DLE CD1 C 24.93 0.00 1 18 6 7 DLE CD2 C 24.92 0.00 1 19 7 8 CYS CA C 55.41 0.00 1 20 7 8 CYS CB C 41.14 0.00 1 21 8 9 DTR CA C 58.34 0.00 1 22 8 9 DTR CB C 29.70 0.00 1 23 8 9 DTR CD1 C 127.14 0.00 1 24 8 9 DTR CE3 C 120.95 0.00 1 25 8 9 DTR CZ2 C 114.75 0.00 1 26 8 9 DTR CZ3 C 122.09 0.00 1 27 8 9 DTR CH2 C 124.71 0.00 1 28 9 10 MET CA C 55.61 0.00 1 29 9 10 MET CB C 27.03 0.01 1 30 9 10 MET CG C 31.31 0.00 1 31 10 11 ASN CA C 53.59 0.00 1 32 10 11 ASN CB C 39.17 0.00 1 33 11 12 GLU CA C 57.31 0.00 1 34 11 12 GLU CB C 30.95 0.00 1 35 11 12 GLU CG C 35.33 0.00 1 36 12 13 TYR CA C 58.08 0.00 1 37 12 13 TYR CB C 38.29 0.02 1 38 12 13 TYR CD1 C 133.15 0.00 3 39 12 13 TYR CD2 C 133.15 0.00 3 40 12 13 TYR CE1 C 118.31 0.00 3 41 12 13 TYR CE2 C 118.31 0.00 3 42 13 14 SER CA C 58.51 0.00 1 43 13 14 SER CB C 63.91 0.00 1 44 14 15 GLY CA C 45.86 0.00 1 45 15 16 TRP CA C 57.67 0.00 1 46 15 16 TRP CB C 29.71 0.01 1 47 15 16 TRP CD1 C 127.14 0.00 1 48 15 16 TRP CE3 C 121.00 0.00 1 49 15 16 TRP CZ2 C 114.70 0.00 1 50 15 16 TRP CZ3 C 122.02 0.00 1 51 15 16 TRP CH2 C 124.68 0.00 1 52 16 17 DCY CA C 55.53 0.00 1 53 16 17 DCY CB C 41.43 0.00 1 54 17 18 MET CA C 56.24 0.00 1 55 17 18 MET CB C 32.70 0.01 1 56 17 18 MET CG C 32.08 0.00 1 57 18 19 DSG CA C 53.47 0.00 1 58 18 19 DSG CB C 38.92 0.00 1 59 19 20 LEU CA C 55.50 0.00 1 60 19 20 LEU CB C 42.44 0.01 1 61 19 20 LEU CG C 27.05 0.00 1 62 19 20 LEU CD1 C 23.32 0.00 1 63 19 20 LEU CD2 C 23.82 0.00 1 64 20 21 DLY CA C 56.55 0.00 1 65 20 21 DLY CB C 32.88 0.01 1 66 20 21 DLY CG C 24.95 0.00 1 67 20 21 DLY CD C 28.99 0.00 1 68 21 22 MET CA C 55.40 0.00 1 69 21 22 MET CB C 32.65 0.01 1 70 21 22 MET CG C 32.18 0.01 1 71 22 23 GLY CA C 45.32 0.00 1 72 23 24 ARG CA C 55.76 0.00 1 73 23 24 ARG CB C 30.80 0.01 1 74 23 24 ARG CG C 27.05 0.00 1 75 23 24 ARG CD C 43.25 0.00 1 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 800 _Mol_system_component_name AP407 _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 8 CYS H 8 CYS HA 7.35 . . . 2 3JHNHA 11 ASN H 11 ASN HA 7.09 . . . 3 3JHNHA 14 SER H 14 SER HA 6.45 . . . 4 3JHNHA 16 TRP H 16 TRP HA 6.76 . . . 5 3JHNHA 18 MET H 18 MET HA 6.34 . . . 6 3JHNHA 19 DSG H 19 DSG HA 7.45 . . . stop_ save_