data_16907 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; The hemagglutinin fusion peptide (H1 subtype) at pH 7.4 ; _BMRB_accession_number 16907 _BMRB_flat_file_name bmr16907.str _Entry_type original _Submission_date 2010-04-29 _Accession_date 2010-04-29 _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 Lorieau Justin L. . 2 Louis John M. . 3 Bax Ad . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 heteronucl_NOE 2 T1_relaxation 2 T2_relaxation 2 H_exch_rates 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 125 "13C chemical shifts" 76 "15N chemical shifts" 23 "T1 relaxation values" 43 "T2 relaxation values" 43 "H exchange rates" 22 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-10-25 update author 'add other data (1H spin-lock)' 2010-07-28 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'The complete influenza hemagglutinin fusion domain adopts a tight helical hairpin arrangement at the lipid:water interface.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 20534508 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Lorieau Justin L. . 2 Louis John M. . 3 Bax Ad . . 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 107 _Journal_issue 25 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 11341 _Page_last 11346 _Year 2010 _Details . loop_ _Keyword 'Fusion peptide' Hemagglutinin 'Membrane protein' NMR stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name HAfp _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label HAfp $HAfp stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_HAfp _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common HAfp _Molecular_mass . _Mol_thiol_state 'not present' loop_ _Biological_function 'Membrane fusion' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 30 _Mol_residue_sequence ; GLFGAIAGFIEGGWTGMIDG WYGSGKKKKD ; loop_ _Residue_seq_code _Residue_label 1 GLY 2 LEU 3 PHE 4 GLY 5 ALA 6 ILE 7 ALA 8 GLY 9 PHE 10 ILE 11 GLU 12 GLY 13 GLY 14 TRP 15 THR 16 GLY 17 MET 18 ILE 19 ASP 20 GLY 21 TRP 22 TYR 23 GLY 24 SER 25 GLY 26 LYS 27 LYS 28 LYS 29 LYS 30 ASP stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-10-28 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value BMRB 26507 HAfp23 100.00 30 100.00 100.00 5.11e-10 PDB 1RD8 "Crystal Sructure Of The 1918 Human H1 Hemagglutinin Precursor (Ha0)" 76.67 182 100.00 100.00 2.25e-07 PDB 1RU7 "1934 Human H1 Hemagglutinin" 76.67 160 100.00 100.00 1.75e-06 PDB 1RVX "1934 H1 Hemagglutinin In Complex With Lsta" 76.67 160 100.00 100.00 1.75e-06 PDB 1RVZ "1934 H1 Hemagglutinin In Complex With Lstc" 76.67 160 100.00 100.00 1.75e-06 PDB 2KXA "The Hemagglutinin Fusion Peptide (H1 Subtype) At Ph 7.4" 100.00 30 100.00 100.00 5.11e-10 PDB 2WRG "Structure Of H1 1918 Hemagglutinin With Human Receptor" 76.67 222 100.00 100.00 2.65e-07 PDB 2WRH "Structure Of H1 Duck Albert Hemagglutinin With Human Receptor" 76.67 222 100.00 100.00 2.39e-07 PDB 3GBN "Crystal Structure Of Fab Cr6261 In Complex With The 1918 H1n1 Influenza Virus Hemagglutinin" 76.67 179 100.00 100.00 1.72e-06 PDB 3LZF "Crystal Structure Of Fab 2d1 In Complex With The 1918 Influenza Virus Hemagglutinin" 76.67 179 100.00 100.00 1.72e-06 PDB 3R2X "Crystal Structure Of The De Novo Designed Binding Protein Hb36.3 In Complex The The 1918 Influenza Virus Hemagglutinin" 76.67 179 100.00 100.00 1.72e-06 PDB 4EEF "Crystal Structure Of The Designed Inhibitor Protein F-Hb80.4 In Complex With The 1918 Influenza Virus Hemagglutinin." 76.67 179 100.00 100.00 1.72e-06 PDB 4F3Z "Crystal Structure Of A Swine H1n2 Influenza Virus Hemagglutinin" 76.67 179 100.00 100.00 2.00e-06 PDB 4GXU "Crystal Structure Of Antibody 1f1 Bound To The 1918 Influenza Hemagglutinin" 76.67 176 100.00 100.00 1.67e-06 PDB 4GXX 'Crystal Structure Of The "avianized" 1918 Influenza Virus Hemagglutinin' 76.67 176 100.00 100.00 1.67e-06 PDB 4JUG "Crystal Structure Of 1918 Pandemic Influenza Virus Hemagglutinin Mutant D225g" 76.67 170 100.00 100.00 3.92e-07 PDB 4JUH "Crystal Structure Of 1918 Pandemic Influenza Virus Hemagglutinin Mutant D225g Complexed With Avian Receptor Analogue Lsta" 76.67 170 100.00 100.00 3.92e-07 PDB 4JUJ "Crystal Structure Of 1918 Pandemic Influenza Virus Hemagglutinin Mutnat D225g Complexed With Human Receptor Analogue Lstc" 76.67 170 100.00 100.00 3.92e-07 PDB 4PY8 "Crystal Structure Of Fab 3.1 In Complex With The 1918 Influenza Virus Hemagglutinin" 76.67 179 100.00 100.00 1.72e-06 PDB 5BNY "Crystal Structure Of Hemagglutinin Of A/chicken/guangdong/s1311/2010 (h6n6)" 76.67 191 100.00 100.00 1.82e-07 PDB 5BQY "Crystal Structure Of Hemagglutinin Of A/chicken/guangdong/s1311/2010 (h6n6) In Complex With Avian-like Receptor Lsta" 76.67 191 100.00 100.00 1.82e-07 PDB 5BQZ "Crystal Structure Of Hemagglutinin Of A/chicken/guangdong/s1311/2010 (h6n6) In Complex With Human-like Receptor Lstc" 76.67 191 100.00 100.00 1.82e-07 DBJ BAA00718 "polyprotein precursor [Influenza A virus (A/swine/Cambridge/1939(H1N1))]" 76.67 565 100.00 100.00 4.54e-08 DBJ BAA00722 "polyprotein precursor, partial [Influenza A virus (A/Yamagata/120/1986(H1N1))]" 76.67 385 100.00 100.00 2.42e-07 DBJ BAA01280 "haemagglutinin [Influenza A virus (A/mallard/Alberta/35/1976(H1N1))]" 76.67 566 100.00 100.00 1.62e-07 DBJ BAA02765 "hemagglutinin [Influenza A virus (A/Bangkok/10/83(H1N1))], partial [Influenza A virus (A/Bangkok/10/1983(H1N1))]" 73.33 141 100.00 100.00 1.57e-06 DBJ BAA02766 "hemagglutinin, partial [Influenza A virus (A/Yamagata/120/1986(H1N1))]" 76.67 141 100.00 100.00 4.86e-07 EMBL CAA24272 "haemagglutinin [Influenza A virus (A/Puerto Rico/8/1934(H1N1))]" 76.67 566 100.00 100.00 8.45e-08 EMBL CAA35094 "haemagglutinin precursor [Influenza A virus (A/CHR/157/83(H1N1))]" 76.67 566 100.00 100.00 1.02e-07 EMBL CAA42444 "polyprotein, partial [Influenza A virus (A/NIB/4/1988(H1N1))]" 53.33 354 100.00 100.00 1.26e-01 EMBL CAA82950 "hemagglutinin precursor [Influenza A virus (A/swine/Germany/2/1981(H1N1))]" 76.67 566 100.00 100.00 1.15e-07 EMBL CAA86560 "hemagglutinin precursor [Influenza A virus (A/swine/Germany/8533/1991(H1N1))]" 76.67 566 100.00 100.00 1.21e-07 GB AAA16879 "hemagglutinin [Influenza A virus (A/duck/WI/1938/80 (H1N1))]" 76.67 566 100.00 100.00 1.15e-07 GB AAA16880 "hemagglutinin [Influenza A virus (A/duck/WI/259/80(H1N1))]" 76.67 566 100.00 100.00 1.07e-07 GB AAA19934 "hemagglutinin [Influenza A virus (A/swine/St-Hyacinthe/106/1991(H1))]" 76.67 566 100.00 100.00 5.90e-08 GB AAA43171 "hemagglutinin [Influenza A virus (A/Leningrad/1954/1(H1N1))]" 76.67 566 100.00 100.00 9.40e-08 GB AAA43172 "hemagglutinin [Influenza A virus (A/Kiev/59/1979(H1N1))]" 76.67 566 100.00 100.00 1.07e-07 PIR HMIV "hemagglutinin precursor - influenza A virus (strain A/PR/8/ 34) [Influenza A virus]" 76.67 566 100.00 100.00 8.45e-08 PIR HMIV17 "hemagglutinin precursor - influenza A virus (strain A/Swine/ Indiana/1726/88 [H1N1]) [Influenza A virus]" 76.67 566 100.00 100.00 7.38e-08 PIR HMIV5 "hemagglutinin precursor - influenza A virus (strain A/WSN/33 [H0N1]) [Influenza A virus]" 76.67 565 100.00 100.00 8.94e-08 PIR HMIVN1 "hemagglutinin precursor - influenza A virus (strain A/swine/ NJ/11/76[H1N1]) [Influenza A virus]" 76.67 566 100.00 100.00 7.38e-08 PIR HMIVSA "hemagglutinin precursor - influenza A virus (strain A/ shearwater/Australia/1/72 [H6N5]) [Influenza A virus]" 76.67 566 100.00 100.00 2.62e-07 PRF 0707273A "hemagglutinin [Influenza A virus]" 76.67 566 100.00 100.00 8.45e-08 REF NP_040980 "haemagglutinin [Influenza A virus (A/Puerto Rico/8/1934(H1N1))]" 76.67 566 100.00 100.00 8.45e-08 REF YP_163736 "HA2 [Influenza A virus (A/Puerto Rico/8/1934(H1N1))]" 76.67 222 100.00 100.00 2.84e-06 SP A3DRP0 "RecName: Full=Hemagglutinin; Contains: RecName: Full=Hemagglutinin HA1 chain; Contains: RecName: Full=Hemagglutinin HA2 chain; " 76.67 566 100.00 100.00 1.15e-07 SP A4GBX7 "RecName: Full=Hemagglutinin; Contains: RecName: Full=Hemagglutinin HA1 chain; Contains: RecName: Full=Hemagglutinin HA2 chain; " 76.67 566 100.00 100.00 1.12e-07 SP A4GCH5 "RecName: Full=Hemagglutinin; Contains: RecName: Full=Hemagglutinin HA1 chain; Contains: RecName: Full=Hemagglutinin HA2 chain; " 76.67 566 100.00 100.00 1.06e-07 SP A4GCI6 "RecName: Full=Hemagglutinin; Contains: RecName: Full=Hemagglutinin HA1 chain; Contains: RecName: Full=Hemagglutinin HA2 chain; " 76.67 566 100.00 100.00 1.15e-07 SP A4GCJ7 "RecName: Full=Hemagglutinin; Contains: RecName: Full=Hemagglutinin HA1 chain; Contains: RecName: Full=Hemagglutinin HA2 chain; " 76.67 566 100.00 100.00 8.62e-08 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _ICTVdb_decimal_code _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Strain _Details $HAfp 'Influenza virus type A' 00.046.0.01 11320 Viruses . 'Influenzavirus A' 'Influenza virus type A' H1 'Hemagglutinin fusion peptide, H1 subtype' 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 $HAfp 'recombinant technology' . Escherichia coli BL21-DE3 pET15b stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_HAfp_H2O_1 _Saveframe_category sample _Sample_type micelle _Details 'The hemagglutinin fusion peptide subtype H1 at pH 7.4 in DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HAfp . mM 0.6 0.8 '[U-13C; U-15N; U-2H]' D2O 7 % . . [U-2H] TRIS 25 mM . . '[U-99% 2H]' DPC . mM 130 180 '[U-99% 2H]' stop_ save_ save_HAfp_D2O_1 _Saveframe_category sample _Sample_type micelle _Details 'The hemagglutinin fusion peptide subtype H1 at pH 7.4 in DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HAfp . mM 0.6 0.8 '[U-13C; U-15N]' TRIS 25 mM . . '[U-99% 2H]' DPC . mM 130 180 '[U-99% 2H]' stop_ save_ save_HAfp_H2O_2 _Saveframe_category sample _Sample_type micelle _Details 'The hemagglutinin fusion peptide subtype H1 at pH 7.4 in DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HAfp . mM 0.6 0.8 '[U-13C; U-15N]' D2O 7 % . . [U-2H] TRIS 25 mM . . '[U-99% 2H]' DPC . mM 130 180 '[U-99% 2H]' stop_ save_ save_HAfp_H2O_3 _Saveframe_category sample _Sample_type micelle _Details 'The hemagglutinin fusion peptide subtype H1 at pH 7.4 in DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HAfp . mM 0.6 0.8 [U-15N] D2O 7 % . . [U-2H] TRIS 25 mM . . '[U-99% 2H]' DPC . mM 130 180 '[U-99% 2H]' stop_ save_ save_HAfp_D2O_2 _Saveframe_category sample _Sample_type micelle _Details 'The hemagglutinin fusion peptide subtype H1 at pH 7.4 in DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HAfp . mM 0.6 0.8 [U-15N] TRIS 25 mM . . '[U-99% 2H]' DPC . mM 130 180 '[U-99% 2H]' stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3.113 loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' 'data analysis' 'peak picking' stop_ _Details . save_ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version 5.0 loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'data analysis' 'peak picking' processing stop_ _Details . save_ save_NMRDraw _Saveframe_category software _Name NMRDraw _Version 5.0 loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'data analysis' 'peak picking' stop_ _Details . save_ save_ModelFree _Saveframe_category software _Name ModelFree _Version 4.2 loop_ _Vendor _Address _Electronic_address Palmer . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_PSVS _Saveframe_category software _Name PSVS _Version 1.4 loop_ _Vendor _Address _Electronic_address 'Bhattacharya and Montelione' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_TALOS _Saveframe_category software _Name TALOS _Version 1.2009.0721.18 loop_ _Vendor _Address _Electronic_address 'Cornilescu, Delaglio and Bax' . . stop_ loop_ _Task 'data analysis' stop_ _Details ; TALOS+ 1.2009.0721.18 ; save_ save_X-PLOR_NIH _Saveframe_category software _Name 'X-PLOR NIH' _Version 2.24 loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task refinement 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_900 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 900 _Details . save_ save_spectrometer_750 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 750 _Details . save_ save_spectrometer_600 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ save_spectrometer_499 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $HAfp_H2O_1 save_ save_2D_1H-13C_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $HAfp_D2O_1 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $HAfp_D2O_1 save_ save_3D_HNCO_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $HAfp_H2O_1 save_ save_3D_HNCA_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $HAfp_H2O_1 save_ save_3D_HN(CO)CA_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _Sample_label $HAfp_H2O_1 save_ save_3D_1H-15N_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $HAfp_H2O_1 save_ save_2D_1H-15N_HSQC_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $HAfp_H2O_1 save_ save_2D_1H-13C_HSQC_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $HAfp_H2O_1 save_ save_3D_HN(CO)CA_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _Sample_label $HAfp_H2O_1 save_ ####################### # Sample conditions # ####################### save_pH_7.4 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . M pH 7.4 . pH pressure 1 . atm temperature 305 . K stop_ save_ save_pH_4.0 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . M pH 4.0 . pH pressure 1 . atm temperature 305 . K 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 C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 na indirect . . . 0.101329118 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-15N HSQC' '2D 1H-13C HSQC' '2D 1H-1H NOESY' '3D HNCO' '3D HNCA' '3D HN(CO)CA' '3D 1H-15N NOESY' stop_ loop_ _Sample_label $HAfp_H2O_1 $HAfp_D2O_1 stop_ _Sample_conditions_label $pH_7.4 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name HAfp _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 GLY HA2 H 3.177 . 2 2 1 1 GLY HA3 H 3.897 . 2 3 1 1 GLY CA C 43.529 . 1 4 2 2 LEU HA H 4.248 . 1 5 2 2 LEU HB2 H 1.844 . 2 6 2 2 LEU HB3 H 1.757 . 2 7 2 2 LEU HD1 H 1.032 . 2 8 2 2 LEU HD2 H 0.938 . 2 9 2 2 LEU HG H 1.617 . 1 10 2 2 LEU C C 177.626 . 1 11 2 2 LEU CA C 59.413 . 1 12 2 2 LEU CB C 42.557 . 1 13 2 2 LEU CD1 C 24.068 . 2 14 2 2 LEU CD2 C 26.109 . 2 15 2 2 LEU CG C 27.452 . 1 16 3 3 PHE H H 9.005 . 1 17 3 3 PHE HA H 4.247 . 1 18 3 3 PHE HB2 H 3.181 . 2 19 3 3 PHE HB3 H 3.181 . 2 20 3 3 PHE HD1 H 7.291 . 3 21 3 3 PHE HD2 H 7.291 . 3 22 3 3 PHE HE1 H 7.314 . 3 23 3 3 PHE HE2 H 7.314 . 3 24 3 3 PHE HZ H 7.252 . 1 25 3 3 PHE C C 179.193 . 1 26 3 3 PHE CA C 61.694 . 1 27 3 3 PHE CB C 37.754 . 1 28 3 3 PHE N N 117.641 . 1 29 4 4 GLY H H 8.778 . 1 30 4 4 GLY HA2 H 3.824 . 2 31 4 4 GLY HA3 H 3.824 . 2 32 4 4 GLY C C 177.492 . 1 33 4 4 GLY CA C 46.540 . 1 34 4 4 GLY N N 107.331 . 1 35 5 5 ALA H H 8.536 . 1 36 5 5 ALA HA H 4.676 . 1 37 5 5 ALA HB H 1.727 . 1 38 5 5 ALA C C 179.009 . 1 39 5 5 ALA CA C 55.069 . 1 40 5 5 ALA CB C 19.562 . 1 41 5 5 ALA N N 126.443 . 1 42 6 6 ILE H H 7.964 . 1 43 6 6 ILE HA H 3.671 . 1 44 6 6 ILE HB H 1.942 . 1 45 6 6 ILE HD1 H 0.823 . 1 46 6 6 ILE HG12 H 1.924 . 2 47 6 6 ILE HG13 H 1.053 . 2 48 6 6 ILE HG2 H 0.936 . 1 49 6 6 ILE C C 177.540 . 1 50 6 6 ILE CA C 65.540 . 1 51 6 6 ILE CB C 38.075 . 1 52 6 6 ILE CD1 C 13.555 . 1 53 6 6 ILE CG1 C 28.980 . 1 54 6 6 ILE CG2 C 17.608 . 1 55 6 6 ILE N N 118.760 . 1 56 7 7 ALA H H 8.306 . 1 57 7 7 ALA HA H 3.954 . 1 58 7 7 ALA HB H 1.373 . 1 59 7 7 ALA C C 180.359 . 1 60 7 7 ALA CA C 55.326 . 1 61 7 7 ALA CB C 18.171 . 1 62 7 7 ALA N N 120.472 . 1 63 8 8 GLY H H 8.333 . 1 64 8 8 GLY HA2 H 3.784 . 2 65 8 8 GLY HA3 H 3.784 . 2 66 8 8 GLY C C 175.888 . 1 67 8 8 GLY CA C 46.334 . 1 68 8 8 GLY N N 105.737 . 1 69 9 9 PHE H H 8.306 . 1 70 9 9 PHE HA H 4.638 . 1 71 9 9 PHE HB2 H 3.196 . 2 72 9 9 PHE HB3 H 3.164 . 2 73 9 9 PHE HD1 H 6.981 . 3 74 9 9 PHE HD2 H 6.981 . 3 75 9 9 PHE HE1 H 6.981 . 3 76 9 9 PHE HE2 H 6.981 . 3 77 9 9 PHE HZ H 6.981 . 1 78 9 9 PHE C C 178.532 . 1 79 9 9 PHE CA C 60.374 . 1 80 9 9 PHE CB C 39.45 . 1 81 9 9 PHE N N 123.393 . 1 82 10 10 ILE H H 7.879 . 1 83 10 10 ILE HA H 3.451 . 1 84 10 10 ILE HB H 2.036 . 1 85 10 10 ILE HD1 H 0.928 . 1 86 10 10 ILE HG12 H 1.981 . 2 87 10 10 ILE HG13 H 1.237 . 2 88 10 10 ILE HG2 H 0.958 . 1 89 10 10 ILE C C 176.952 . 1 90 10 10 ILE CA C 65.122 . 1 91 10 10 ILE CB C 37.966 . 1 92 10 10 ILE CD1 C 13.789 . 1 93 10 10 ILE CG1 C 29.636 . 1 94 10 10 ILE CG2 C 17.504 . 1 95 10 10 ILE N N 119.279 . 1 96 11 11 GLU H H 7.788 . 1 97 11 11 GLU HA H 4.179 . 1 98 11 11 GLU HB2 H 2.021 . 2 99 11 11 GLU HB3 H 2.021 . 2 100 11 11 GLU HG2 H 2.300 . 2 101 11 11 GLU HG3 H 2.215 . 2 102 11 11 GLU C C 178.407 . 1 103 11 11 GLU CA C 58.337 . 1 104 11 11 GLU CB C 30.953 . 1 105 11 11 GLU CG C 36.384 . 1 106 11 11 GLU N N 115.573 . 1 107 12 12 GLY H H 8.469 . 1 108 12 12 GLY HA2 H 4.564 . 2 109 12 12 GLY HA3 H 3.653 . 2 110 12 12 GLY C C 175.927 . 1 111 12 12 GLY CA C 45.883 . 1 112 12 12 GLY N N 105.522 . 1 113 13 13 GLY H H 8.385 . 1 114 13 13 GLY HA2 H 3.054 . 2 115 13 13 GLY HA3 H 4.026 . 2 116 13 13 GLY C C 174.068 . 1 117 13 13 GLY CA C 45.325 . 1 118 13 13 GLY N N 112.314 . 1 119 14 14 TRP H H 9.095 . 1 120 14 14 TRP HA H 4.430 . 1 121 14 14 TRP HB2 H 3.520 . 2 122 14 14 TRP HB3 H 3.426 . 2 123 14 14 TRP HD1 H 7.362 . 1 124 14 14 TRP HE1 H 10.743 . 1 125 14 14 TRP HE3 H 7.610 . 1 126 14 14 TRP HH2 H 6.998 . 1 127 14 14 TRP HZ2 H 7.485 . 1 128 14 14 TRP HZ3 H 6.897 . 1 129 14 14 TRP C C 177.620 . 1 130 14 14 TRP CA C 61.345 . 1 131 14 14 TRP CB C 29.891 . 1 132 14 14 TRP N N 124.653 . 1 133 14 14 TRP NE1 N 130.639 . 1 134 15 15 THR H H 8.616 . 1 135 15 15 THR HA H 3.947 . 1 136 15 15 THR HB H 4.207 . 1 137 15 15 THR HG2 H 1.332 . . 138 15 15 THR C C 176.832 . 1 139 15 15 THR CA C 66.218 . 1 140 15 15 THR CB C 68.526 . 1 141 15 15 THR CG2 C 22.157 . 1 142 15 15 THR N N 110.877 . 1 143 16 16 GLY H H 7.225 . 1 144 16 16 GLY HA2 H 3.868 . 2 145 16 16 GLY HA3 H 3.631 . 2 146 16 16 GLY C C 177.020 . 1 147 16 16 GLY CA C 46.744 . 1 148 16 16 GLY N N 108.970 . 1 149 17 17 MET H H 8.520 . 1 150 17 17 MET HA H 4.579 . 1 151 17 17 MET HB2 H 2.648 . 2 152 17 17 MET HB3 H 2.114 . 2 153 17 17 MET HG2 H 2.500 . 2 154 17 17 MET HG3 H 2.157 . 2 155 17 17 MET C C 177.611 . 1 156 17 17 MET CA C 58.632 . 1 157 17 17 MET CB C 34.056 . 1 158 17 17 MET CG C 31.721 . 1 159 17 17 MET N N 125.013 . 1 160 18 18 ILE H H 7.857 . 1 161 18 18 ILE HA H 3.656 . 1 162 18 18 ILE HB H 2.041 . 1 163 18 18 ILE HD1 H 0.674 . 1 164 18 18 ILE HG12 H 1.523 . 2 165 18 18 ILE HG13 H 1.070 . 2 166 18 18 ILE HG2 H 1.144 . 1 167 18 18 ILE C C 178.075 . 1 168 18 18 ILE CA C 64.513 . 1 169 18 18 ILE CB C 37.425 . 1 170 18 18 ILE CD1 C 12.168 . 1 171 18 18 ILE CG1 C 28.392 . 1 172 18 18 ILE CG2 C 18.051 . 1 173 18 18 ILE N N 119.813 . 1 174 19 19 ASP H H 8.041 . 1 175 19 19 ASP HA H 4.589 . 1 176 19 19 ASP HB2 H 2.708 . 2 177 19 19 ASP HB3 H 2.622 . 2 178 19 19 ASP C C 179.897 . 1 179 19 19 ASP CA C 57.407 . 1 180 19 19 ASP CB C 40.484 . 1 181 19 19 ASP N N 118.945 . 1 182 20 20 GLY H H 8.352 . 1 183 20 20 GLY HA2 H 3.817 . 2 184 20 20 GLY HA3 H 3.701 . 2 185 20 20 GLY C C 176.088 . 1 186 20 20 GLY CA C 45.965 . 1 187 20 20 GLY N N 107.496 . 1 188 21 21 TRP H H 8.587 . 1 189 21 21 TRP HA H 4.465 . 1 190 21 21 TRP HB2 H 3.304 . 2 191 21 21 TRP HB3 H 3.138 . 2 192 21 21 TRP HD1 H 5.472 . 1 193 21 21 TRP HE1 H 10.374 . 1 194 21 21 TRP HE3 H 7.168 . 1 195 21 21 TRP HH2 H 6.988 . 1 196 21 21 TRP HZ2 H 7.407 . 1 197 21 21 TRP HZ3 H 6.721 . 1 198 21 21 TRP C C 177.123 . 1 199 21 21 TRP CA C 59.817 . 1 200 21 21 TRP CB C 29.747 . 1 201 21 21 TRP N N 123.763 . 1 202 21 21 TRP NE1 N 129.889 . 1 203 22 22 TYR H H 7.767 . 1 204 22 22 TYR HA H 4.127 . 1 205 22 22 TYR HB2 H 3.234 . 2 206 22 22 TYR HB3 H 2.946 . 2 207 22 22 TYR HD1 H 7.436 . 3 208 22 22 TYR HD2 H 7.436 . 3 209 22 22 TYR HE1 H 6.991 . 3 210 22 22 TYR HE2 H 6.991 . 3 211 22 22 TYR C C 177.574 . 1 212 22 22 TYR CA C 60.633 . 1 213 22 22 TYR CB C 38.926 . 1 214 22 22 TYR N N 113.074 . 1 215 23 23 GLY H H 8.074 . 1 216 23 23 GLY HA2 H 4.067 . 2 217 23 23 GLY HA3 H 3.998 . 2 218 23 23 GLY CA C 46.040 . 1 219 23 23 GLY N N 108.785 . 1 220 24 24 SER HA H 4.461 . 1 221 24 24 SER HB2 H 3.923 . 2 222 24 24 SER HB3 H 3.823 . 2 223 24 24 SER CA C 63.835 . 1 224 24 24 SER CB C 63.857 . 1 stop_ save_ save_T1_pH7.4 _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $HAfp_H2O_1 stop_ _Sample_conditions_label $pH_7.4 _Spectrometer_frequency_1H 600 _T1_coherence_type Nz _T1_value_units s _Mol_system_component_name HAfp _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 3 PHE N 0.69 0.01 2 4 GLY N 0.65 0.02 3 5 ALA N 0.69 0 4 6 ILE N 0.7 0.02 5 7 ALA N 0.7 0.01 6 8 GLY N 0.72 0 7 9 PHE N 0.73 0 8 10 ILE N 0.71 0.02 9 11 GLU N 0.72 0 10 12 GLY N 0.79 0.01 11 13 GLY N 0.7 0 12 14 TRP N 0.71 0.02 13 15 THR N 0.74 0 14 16 GLY N 0.72 0.01 15 17 MET N 0.68 0.01 16 18 ILE N 0.7 0.01 17 19 ASP N 0.71 0.01 18 20 GLY N 0.7 0 19 21 TRP N 0.71 0 20 22 TYR N 0.7 0.01 21 23 GLY N 0.71 0.01 stop_ save_ save_T1_pH4.0 _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $HAfp_H2O_1 stop_ _Sample_conditions_label $pH_4.0 _Spectrometer_frequency_1H 600 _T1_coherence_type Nz _T1_value_units s _Mol_system_component_name HAfp _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 2 LEU N 0.78 0.01 2 3 PHE N 0.74 0.01 3 4 GLY N 0.74 0.01 4 5 ALA N 0.72 0.01 5 6 ILE N 0.77 0.01 6 7 ALA N 0.73 0.01 7 8 GLY N 0.74 0.01 8 9 PHE N 0.74 0.01 9 10 ILE N 0.73 0.01 10 11 GLU N 0.77 0.02 11 12 GLY N 0.87 0.01 12 13 GLY N 0.74 0.02 13 14 TRP N 0.79 0.05 14 15 THR N 0.78 0.02 15 16 GLY N 0.73 0.04 16 17 MET N 0.76 0.01 17 18 ILE N 0.76 0.01 18 19 ASP N 0.72 0.01 19 20 GLY N 0.76 0.01 20 21 TRP N 0.76 0.02 21 22 TYR N 0.71 0.01 22 23 GLY N 0.74 0.01 stop_ save_ save_T2_pH7.4 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $HAfp_H2O_1 stop_ _Sample_conditions_label $pH_7.4 _Spectrometer_frequency_1H 600 _T2_coherence_type Nz _T2_value_units s _Mol_system_component_name HAfp _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 3 PHE N 0.100 0.001 . . 2 4 GLY N 0.091 0.001 . . 3 5 ALA N 0.085 0.002 . . 4 6 ILE N 0.094 0.002 . . 5 7 ALA N 0.093 0.001 . . 6 8 GLY N 0.091 0.000 . . 7 9 PHE N 0.089 0.002 . . 8 10 ILE N 0.092 0.002 . . 9 11 GLU N 0.089 0.001 . . 10 12 GLY N 0.098 0.001 . . 11 13 GLY N 0.090 0.002 . . 12 14 TRP N 0.095 0.002 . . 13 15 THR N 0.095 0.001 . . 14 16 GLY N 0.092 0.001 . . 15 17 MET N 0.082 0.001 . . 16 18 ILE N 0.093 0.000 . . 17 19 ASP N 0.094 0.001 . . 18 20 GLY N 0.095 0.002 . . 19 21 TRP N 0.089 0.001 . . 20 22 TYR N 0.090 0.001 . . 21 23 GLY N 0.106 0.001 . . stop_ save_ save_T2_pH4.0 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $HAfp_H2O_1 stop_ _Sample_conditions_label $pH_4.0 _Spectrometer_frequency_1H 600 _T2_coherence_type Nz _T2_value_units s _Mol_system_component_name HAfp _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 2 LEU N 0.071 0.002 . . 2 3 PHE N 0.086 0.004 . . 3 4 GLY N 0.090 0.002 . . 4 5 ALA N 0.077 0.002 . . 5 6 ILE N 0.094 0.002 . . 6 7 ALA N 0.082 0.001 . . 7 8 GLY N 0.087 0.002 . . 8 9 PHE N 0.084 0.001 . . 9 10 ILE N 0.085 0.002 . . 10 11 GLU N 0.064 0.001 . . 11 12 GLY N 0.088 0.000 . . 12 13 GLY N 0.071 0.002 . . 13 14 TRP N 0.068 0.002 . . 14 15 THR N 0.090 0.001 . . 15 16 GLY N 0.086 0.001 . . 16 17 MET N 0.063 0.002 . . 17 18 ILE N 0.083 0.001 . . 18 19 ASP N 0.088 0.001 . . 19 20 GLY N 0.090 0.001 . . 20 21 TRP N 0.081 0.002 . . 21 22 TYR N 0.071 0.001 . . 22 23 GLY N 0.110 0.002 . . stop_ save_ save_heteronuclear_noe_pH7.4 _Saveframe_category heteronuclear_NOE _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label . stop_ _Sample_conditions_label $pH_7.4 _Spectrometer_frequency_1H 600 _Mol_system_component_name HAfp _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'peak height' _NOE_reference_value 2e6 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 3 PHE 0.791 0.043 4 GLY 0.826 0.049 5 ALA 0.733 0.033 6 ILE 0.727 0.037 7 ALA 0.707 0.031 8 GLY 0.769 0.040 9 PHE 0.681 0.035 10 ILE 0.710 0.035 11 GLU 0.703 0.031 12 GLY 0.713 0.041 13 GLY 0.695 0.035 14 TRP 0.770 0.052 15 THR 0.699 0.029 16 GLY 0.719 0.033 17 MET 0.770 0.044 18 ILE 0.783 0.037 19 ASP 0.721 0.028 20 GLY 0.740 0.038 21 TRP 0.732 0.036 22 TYR 0.735 0.038 23 GLY 0.642 0.029 stop_ save_ save_heteronuclear_noe_pH4.0 _Saveframe_category heteronuclear_NOE _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label . stop_ _Sample_conditions_label $pH_7.4 _Spectrometer_frequency_1H 600 _Mol_system_component_name HAfp _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'peak height' _NOE_reference_value 3e6 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 2 LEU 0.68 0.036 3 PHE 0.713 0.022 4 GLY 0.727 0.029 5 ALA 0.766 0.022 6 ILE 0.722 0.021 7 ALA 0.696 0.019 8 GLY 0.754 0.024 9 PHE 0.745 0.024 10 ILE 0.702 0.023 11 GLU 0.749 0.028 12 GLY 0.635 0.024 13 GLY 0.648 0.021 14 TRP 0.697 0.036 15 THR 0.712 0.026 16 GLY 0.654 0.025 17 MET 0.725 0.039 18 ILE 0.780 0.023 19 ASP 0.720 0.017 20 GLY 0.664 0.022 21 TRP 0.708 0.026 22 TYR 0.755 0.031 23 GLY 0.560 0.013 stop_ save_ save_HX_pH7.4 _Saveframe_category H_exchange_rates _Details . loop_ _Sample_label $HAfp_H2O_1 stop_ _Sample_conditions_label $pH_7.4 _H_exchange_rate_units s-1 _Mol_system_component_name HAfp _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _H_exchange_rate_value _H_exchange_rate_min_value _H_exchange_rate_max_value _H_exchange_rate_value_error 2 LEU H 47.8 . . . 3 PHE H 1.52 . . . 4 GLY H 1.9 . . . 5 ALA H 0.49 . . . 6 ILE H 0.12 . . . 7 ALA H 0 . . . 8 GLY H 0 . . . 9 PHE H 0 . . . 10 ILE H 0 . . . 11 GLU H 0 . . . 12 GLY H 0.28 . . . 13 GLY H 0.4 . . . 14 TRP H 2.76 . . . 15 THR H 1.15 . . . 16 GLY H 0.52 . . . 17 MET H 0.16 . . . 18 ILE H 0 . . . 19 ASP H 0 . . . 20 GLY H 0.17 . . . 21 TRP H 0.19 . . . 22 TYR H 0.5 . . . 23 GLY H 1.79 . . . stop_ save_