data_30572 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Dimer-of-dimer amyloid fibril structure of glucagon ; _BMRB_accession_number 30572 _BMRB_flat_file_name bmr30572.str _Entry_type original _Submission_date 2019-02-14 _Accession_date 2019-02-14 _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 Gelenter M. D. . 2 Smith K. J. . 3 Liao S. Y. . 4 Mandala V. S. . 5 Dregni A. J. . 6 Lamm M. S. . 7 Tian Y. . . 8 Wei X. . . 9 Pochan D. J. . 10 Tucker T. J. . 11 Su Y. . . 12 Hong M. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 306 "15N chemical shifts" 86 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-07-08 update BMRB 'update entry citation' 2019-05-28 original author 'original release' stop_ _Original_release_date 2019-03-27 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; The peptide hormone glucagon forms amyloid fibrils with two coexisting beta-strand conformations ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 31235909 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Gelenter M. D. . 2 Smith K. J. . 3 Liao S. Y. . 4 Mandala V. S. . 5 Dregni A. J. . 6 Lamm M. S. . 7 Tian Y. . . 8 Wei X. . . 9 Pochan D. J. . 10 Tucker T. J. . 11 Su Y. . . 12 Hong M. . . stop_ _Journal_abbreviation 'Nat. Struc. Mol. Biol.' _Journal_name_full 'Nature Structural & Molecular Biology' _Journal_volume 26 _Journal_issue 7 _Journal_ISSN 1545-9985 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 592 _Page_last 598 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Glucagon _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'entity_1, 1' $entity_1 'entity_1, 2' $entity_1 'entity_1, 3' $entity_1 'entity_1, 4' $entity_1 'entity_1, 5' $entity_1 'entity_1, 6' $entity_1 'entity_1, 7' $entity_1 'entity_1, 8' $entity_1 'entity_1, 9' $entity_1 'entity_1, 10' $entity_1 'entity_1, 11' $entity_1 'entity_1, 12' $entity_1 'entity_1, 13' $entity_1 'entity_1, 14' $entity_1 'entity_1, 15' $entity_1 'entity_1, 16' $entity_1 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 3486.781 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 29 _Mol_residue_sequence ; HSQGTFTSDYSKYLDSRRAQ DFVQWLMNT ; loop_ _Residue_seq_code _Residue_label 1 HIS 2 SER 3 GLN 4 GLY 5 THR 6 PHE 7 THR 8 SER 9 ASP 10 TYR 11 SER 12 LYS 13 TYR 14 LEU 15 ASP 16 SER 17 ARG 18 ARG 19 ALA 20 GLN 21 ASP 22 PHE 23 VAL 24 GLN 25 TRP 26 LEU 27 MET 28 ASN 29 THR stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1 Human 9606 Eukaryota Metazoa Homo sapiens 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 $entity_1 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type 'fibrous protein' _Details '0.1 mg/uL {U-13C; U-15N]-G4,S8,L14,A19,V23 Glucagon, water' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.1 mg/uL '{U-13C; U-15N]-G4,S8,L14,A19,V23' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type 'fibrous protein' _Details '0.1 mg/uL {U-13C; U-15N]-S2,Q3,G4,T5,Q24,W25,L26,M27,N28 Glucagon, water' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.1 mg/uL '{U-13C; U-15N]-S2,Q3,G4,T5,Q24,W25,L26,M27,N28' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type 'fibrous protein' _Details '0.1 mg/uL {U-13C; U-15N]-T5,F6,T7,S8,D9,Y10,S11,A19,Q20,D21,F22,V23,Q24 Glucagon, water' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.1 mg/uL '{U-13C; U-15N]-T5,F6,T7,S8,D9,Y10,S11,A19,Q20,D21,F22,V23,Q24' stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type 'fibrous protein' _Details '0.1 mg/uL {U-13C; U-15N]-S11,K12,Y13,L14,D15,S16,R17,R18,A19 Glucagon, water' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.1 mg/uL '{U-13C; U-15N]-S11,K12,Y13,L14,D15,S16,R17,R18,A19' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CYANA _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task refinement 'structure calculation' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name SPARKY _Version 'NMRFAM-SPARKY 1.412' loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name TOPSPIN _Version 3.5 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceII _Field_strength 800 _Details . save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII-HD _Field_strength 600 _Details . save_ save_NMR_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 900 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_13C-13C_CORD_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C CORD' _Sample_label $sample_1 save_ save_2D_13C-13C_CORD_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C CORD' _Sample_label $sample_2 save_ save_2D_15N-13C_PERSPIRATION-CP_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 15N-13C PERSPIRATION-CP' _Sample_label $sample_2 save_ save_2D_13C-13C_PAR_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C PAR' _Sample_label $sample_2 save_ save_2D_CHHC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CHHC' _Sample_label $sample_2 save_ save_2D_15N-13C_NCCX_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 15N-13C NCCX' _Sample_label $sample_2 save_ save_3D_15N-13C-13C_NCCX_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 15N-13C-13C NCCX' _Sample_label $sample_4 save_ save_3D_15N-13C-13C_NCACX_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 15N-13C-13C NCACX' _Sample_label $sample_3 save_ save_3D_15N-13C-13C_NCOCX_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 15N-13C-13C NCOCX' _Sample_label $sample_3 save_ save_2D_15N-13C_NCA_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 15N-13C NCA' _Sample_label $sample_1 save_ save_2D_13C-13C_CORD_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C CORD' _Sample_label $sample_2 save_ save_2D_CHHC_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CHHC' _Sample_label $sample_4 save_ save_2D_13C-13C_CORD_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C CORD' _Sample_label $sample_4 save_ save_2D-13C-13C_CORD_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D-13C-13C CORD' _Sample_label $sample_4 save_ save_2D_13C-13C_CORD_15 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C CORD' _Sample_label $sample_3 save_ save_2D_13C-13C_PDSD_16 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 13C-13C PDSD' _Sample_label $sample_3 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.01 0.002 M pH 2.0 0.1 pH pressure 1 0.01 atm temperature 293 0.2 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Saveframe_category chemical_shift_reference _Details '13C chemical shifts are reported on the TMS scale and 15N chemical shifts are reported on the liquid ammonia scale' 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 adamantane C 13 'methyl carbons' ppm 38.48 external direct . . . 0.25 NAV N 15 nitrogen ppm 122.00 external direct . . . 0.1 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_chemical_shifts_1_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 13C-13C CORD' '2D 15N-13C PERSPIRATION-CP' '2D 13C-13C PAR' '2D CHHC' '2D 15N-13C NCCX' '3D 15N-13C-13C NCCX' '3D 15N-13C-13C NCACX' '3D 15N-13C-13C NCOCX' '2D 15N-13C NCA' '2D-13C-13C CORD' '2D 13C-13C PDSD' stop_ loop_ _Sample_label $sample_1 $sample_2 $sample_4 $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name 'entity_1, 1' _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 HIS C C 168.5 0.2 1 2 1 1 HIS CA C 53.9 0.2 1 3 1 1 HIS CB C 27.6 0.2 1 4 1 1 HIS CG C 127.6 0.2 1 5 1 1 HIS CD2 C 119.4 0.2 1 6 1 1 HIS CE1 C 135.4 0.2 1 7 1 1 HIS N N 38.7 0.2 1 8 1 1 HIS ND1 N 180.4 0.2 . 9 1 1 HIS NE2 N 174.1 0.2 . 10 2 2 SER C C 171.0 0.2 1 11 2 2 SER CA C 56.2 0.2 1 12 2 2 SER CB C 63.3 0.2 1 13 2 2 SER N N 118.6 0.2 1 14 3 3 GLN C C 172.0 0.2 1 15 3 3 GLN CA C 53.6 0.2 1 16 3 3 GLN CB C 30.5 0.2 1 17 3 3 GLN CG C 32.0 0.2 1 18 3 3 GLN CD C 179.2 0.2 1 19 3 3 GLN N N 122.3 0.2 1 20 3 3 GLN NE2 N 107.1 0.2 1 21 4 4 GLY C C 170.5 0.2 1 22 4 4 GLY CA C 43.8 0.2 1 23 4 4 GLY N N 111.3 0.2 1 24 5 5 THR C C 170.2 0.2 1 25 5 5 THR CA C 58.4 0.2 1 26 5 5 THR CB C 68.1 0.2 1 27 5 5 THR CG2 C 20.7 0.2 1 28 5 5 THR N N 115.8 0.2 1 29 6 6 PHE C C 172.0 0.2 1 30 6 6 PHE CA C 55.0 0.2 1 31 6 6 PHE CB C 41.0 0.2 1 32 6 6 PHE CG C 136.6 0.2 1 33 6 6 PHE CD1 C 129.1 0.2 3 34 6 6 PHE CD2 C 129.1 0.2 3 35 6 6 PHE CE1 C 130.2 0.2 3 36 6 6 PHE CE2 C 130.2 0.2 3 37 6 6 PHE CZ C 128.1 0.2 1 38 6 6 PHE N N 126.2 0.2 1 39 7 7 THR C C 169.1 0.2 1 40 7 7 THR CA C 60.0 0.2 1 41 7 7 THR CB C 71.6 0.2 1 42 7 7 THR CG2 C 17.4 0.2 1 43 7 7 THR N N 124.0 0.2 1 44 8 8 SER C C 171.1 0.2 1 45 8 8 SER CA C 54.8 0.2 1 46 8 8 SER CB C 65.0 0.2 1 47 8 8 SER N N 117.0 0.2 1 48 9 9 ASP C C 172.0 0.2 1 49 9 9 ASP CA C 49.5 0.2 1 50 9 9 ASP CB C 38.8 0.2 1 51 9 9 ASP CG C 174.4 0.2 1 52 9 9 ASP N N 121.5 0.2 1 53 10 10 TYR C C 172.0 0.2 1 54 10 10 TYR CA C 54.8 0.2 1 55 10 10 TYR CB C 40.1 0.2 1 56 10 10 TYR CG C 129.5 0.2 1 57 10 10 TYR CD1 C 130.6 0.2 3 58 10 10 TYR CD2 C 130.6 0.2 3 59 10 10 TYR CE1 C 116.1 0.2 3 60 10 10 TYR CE2 C 116.1 0.2 3 61 10 10 TYR CZ C 154.8 0.2 1 62 10 10 TYR N N 130.0 0.2 1 63 11 11 SER C C 169.7 0.2 1 64 11 11 SER CA C 54.7 0.2 1 65 11 11 SER CB C 64.5 0.2 1 66 11 11 SER N N 122.2 0.2 1 67 12 12 LYS C C 171.8 0.2 1 68 12 12 LYS CA C 53.6 0.2 1 69 12 12 LYS CB C 34.9 0.2 1 70 12 12 LYS CG C 23.3 0.2 1 71 12 12 LYS CD C 27.8 0.2 1 72 12 12 LYS CE C 40.4 0.2 1 73 12 12 LYS N N 124.0 0.2 1 74 12 12 LYS NZ N 33.7 0.2 1 75 13 13 TYR C C 172.2 0.2 1 76 13 13 TYR CA C 54.6 0.2 1 77 13 13 TYR CB C 39.3 0.2 1 78 13 13 TYR CG C 128.4 0.2 1 79 13 13 TYR CD1 C 130.9 0.2 3 80 13 13 TYR CD2 C 130.9 0.2 3 81 13 13 TYR CE1 C 116.0 0.2 3 82 13 13 TYR CE2 C 116.0 0.2 3 83 13 13 TYR CZ C 155.5 0.2 1 84 13 13 TYR N N 125.3 0.2 1 85 14 14 LEU C C 173.6 0.2 1 86 14 14 LEU CA C 52.9 0.2 1 87 14 14 LEU CB C 43.4 0.2 1 88 14 14 LEU CG C 25.9 0.2 1 89 14 14 LEU CD1 C 23.6 0.2 2 90 14 14 LEU CD2 C 23.4 0.2 2 91 14 14 LEU N N 127.7 0.2 1 92 15 15 ASP C C 171.9 0.2 1 93 15 15 ASP CA C 51.1 0.2 1 94 15 15 ASP CB C 41.1 0.2 1 95 15 15 ASP CG C 175.4 0.2 1 96 15 15 ASP N N 120.9 0.2 1 97 16 16 SER C C 171.9 0.2 1 98 16 16 SER CA C 55.2 0.2 1 99 16 16 SER CB C 64.4 0.2 1 100 16 16 SER N N 116.8 0.2 1 101 17 17 ARG C C 173.4 0.2 1 102 17 17 ARG CA C 53.0 0.2 1 103 17 17 ARG CB C 32.5 0.2 1 104 17 17 ARG CG C 25.6 0.2 1 105 17 17 ARG CD C 42.1 0.2 1 106 17 17 ARG CZ C 158.3 0.2 1 107 17 17 ARG N N 126.3 0.2 1 108 17 17 ARG NE N 85.6 0.2 1 109 17 17 ARG NH1 N 72.5 0.2 2 110 17 17 ARG NH2 N 72.5 0.2 2 111 18 18 ARG C C 172.0 0.2 1 112 18 18 ARG CA C 53.2 0.2 1 113 18 18 ARG CB C 32.9 0.2 1 114 18 18 ARG CG C 26.2 0.2 1 115 18 18 ARG CD C 42.0 0.2 1 116 18 18 ARG CZ C 158.3 0.2 1 117 18 18 ARG N N 127.5 0.2 1 118 18 18 ARG NE N 85.6 0.2 1 119 18 18 ARG NH1 N 72.5 0.2 2 120 18 18 ARG NH2 N 72.5 0.2 2 121 19 19 ALA C C 174.1 0.2 1 122 19 19 ALA CA C 49.2 0.2 1 123 19 19 ALA CB C 19.9 0.2 1 124 19 19 ALA N N 128.9 0.2 1 125 20 20 GLN C C 171.3 0.2 1 126 20 20 GLN CA C 53.0 0.2 1 127 20 20 GLN CB C 30.3 0.2 1 128 20 20 GLN CG C 32.0 0.2 1 129 20 20 GLN CD C 178.9 0.2 1 130 20 20 GLN N N 120.8 0.2 1 131 20 20 GLN NE2 N 112.4 0.2 1 132 21 21 ASP C C 171.6 0.2 1 133 21 21 ASP CA C 50.7 0.2 1 134 21 21 ASP CB C 40.0 0.2 1 135 21 21 ASP CG C 174.2 0.2 1 136 21 21 ASP N N 124.5 0.2 1 137 22 22 PHE C C 172.9 0.2 1 138 22 22 PHE CA C 50.4 0.2 1 139 22 22 PHE CB C 41.4 0.2 1 140 22 22 PHE CG C 137.1 0.2 1 141 22 22 PHE CD1 C 130.4 0.2 3 142 22 22 PHE CD2 C 130.4 0.2 3 143 22 22 PHE CE1 C 129.0 0.2 3 144 22 22 PHE CE2 C 129.0 0.2 3 145 22 22 PHE CZ C 127.8 0.2 1 146 22 22 PHE N N 130.2 0.2 1 147 23 23 VAL C C 170.8 0.2 1 148 23 23 VAL CA C 58.2 0.2 1 149 23 23 VAL CB C 34.0 0.2 1 150 23 23 VAL CG1 C 20.4 0.2 2 151 23 23 VAL CG2 C 19.0 0.2 2 152 23 23 VAL N N 128.9 0.2 1 153 24 24 GLN C C 171.1 0.2 1 154 24 24 GLN CA C 52.6 0.2 1 155 24 24 GLN CB C 31.8 0.2 1 156 24 24 GLN CG C 33.7 0.2 1 157 24 24 GLN CD C 178.4 0.2 1 158 24 24 GLN N N 125.1 0.2 1 159 24 24 GLN NE2 N 108.3 0.2 1 160 25 25 TRP C C 170.9 0.2 1 161 25 25 TRP CA C 52.7 0.2 1 162 25 25 TRP CB C 31.5 0.2 1 163 25 25 TRP CG C 109.2 0.2 1 164 25 25 TRP CD1 C 122.8 0.2 1 165 25 25 TRP CD2 C 130.6 0.2 1 166 25 25 TRP CE2 C 136.0 0.2 1 167 25 25 TRP CE3 C 117.7 0.2 1 168 25 25 TRP CZ2 C 111.0 0.2 1 169 25 25 TRP CZ3 C 119.4 0.2 1 170 25 25 TRP CH2 C 121.7 0.2 1 171 25 25 TRP N N 122.0 0.2 1 172 25 25 TRP NE1 N 129.4 0.2 1 173 26 26 LEU C C 174.2 0.2 1 174 26 26 LEU CA C 52.0 0.2 1 175 26 26 LEU CB C 41.7 0.2 1 176 26 26 LEU CG C 26.2 0.2 1 177 26 26 LEU CD1 C 23.9 0.2 2 178 26 26 LEU CD2 C 21.3 0.2 2 179 26 26 LEU N N 118.3 0.2 1 180 27 27 MET C C 172.8 0.2 1 181 27 27 MET CA C 53.2 0.2 1 182 27 27 MET CB C 34.2 0.2 1 183 27 27 MET CG C 30.7 0.2 1 184 27 27 MET CE C 14.8 0.2 1 185 27 27 MET N N 121.4 0.2 1 186 28 28 ASN C C 172.3 0.2 1 187 28 28 ASN CA C 51.0 0.2 1 188 28 28 ASN CB C 39.8 0.2 1 189 28 28 ASN CG C 175.1 0.2 1 190 28 28 ASN N N 116.4 0.2 1 191 28 28 ASN ND2 N 113.6 0.2 1 192 29 29 THR C C 176.7 0.2 1 193 29 29 THR CA C 60.1 0.2 1 194 29 29 THR CB C 68.5 0.2 1 195 29 29 THR CG2 C 20.9 0.2 1 196 29 29 THR N N 114.7 0.2 1 stop_ save_ save_assigned_chemical_shifts_1_9 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 13C-13C CORD' '2D 15N-13C PERSPIRATION-CP' '2D 13C-13C PAR' '2D CHHC' '2D 15N-13C NCCX' '3D 15N-13C-13C NCCX' '3D 15N-13C-13C NCACX' '3D 15N-13C-13C NCOCX' '2D 15N-13C NCA' '2D-13C-13C CORD' '2D 13C-13C PDSD' stop_ loop_ _Sample_label $sample_1 $sample_2 $sample_4 $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name 'entity_1, 9' _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 1 101 1 HIS C C 168.9 0.2 1 2 101 1 HIS CA C 53.2 0.2 1 3 101 1 HIS CB C 27.1 0.2 1 4 101 1 HIS CG C 126.9 0.2 1 5 101 1 HIS CD2 C 119.3 0.2 1 6 101 1 HIS CE1 C 135.4 0.2 1 7 101 1 HIS N N 38.7 0.2 1 8 101 1 HIS ND1 N 179.9 0.2 . 9 101 1 HIS NE2 N 174.1 0.2 . 10 102 2 SER C C 170.9 0.2 1 11 102 2 SER CA C 55.8 0.2 1 12 102 2 SER CB C 63.9 0.2 1 13 102 2 SER N N 118.1 0.2 1 14 103 3 GLN C C 172.6 0.2 1 15 103 3 GLN CA C 54.0 0.2 1 16 103 3 GLN CB C 30.9 0.2 1 17 103 3 GLN CG C 32.8 0.2 1 18 103 3 GLN CD C 178.7 0.2 1 19 103 3 GLN N N 120.5 0.2 1 20 103 3 GLN NE2 N 109.2 0.2 1 21 104 4 GLY C C 169.6 0.2 1 22 104 4 GLY CA C 43.3 0.2 1 23 104 4 GLY N N 111.3 0.2 1 24 105 5 THR C C 171.1 0.2 1 25 105 5 THR CA C 58.0 0.2 1 26 105 5 THR CB C 69.7 0.2 1 27 105 5 THR CG2 C 19.5 0.2 1 28 105 5 THR N N 116.1 0.2 1 29 106 6 PHE C C 171.1 0.2 1 30 106 6 PHE CA C 56.3 0.2 1 31 106 6 PHE CB C 41.5 0.2 1 32 106 6 PHE CG C 135.8 0.2 1 33 106 6 PHE CD1 C 129.1 0.2 3 34 106 6 PHE CD2 C 129.1 0.2 3 35 106 6 PHE CE1 C 130.2 0.2 3 36 106 6 PHE CE2 C 130.2 0.2 3 37 106 6 PHE CZ C 128.1 0.2 1 38 106 6 PHE N N 125.5 0.2 1 39 107 7 THR C C 169.6 0.2 1 40 107 7 THR CA C 59.7 0.2 1 41 107 7 THR CB C 70.6 0.2 1 42 107 7 THR CG2 C 19.4 0.2 1 43 107 7 THR N N 123.9 0.2 1 44 108 8 SER C C 171.3 0.2 1 45 108 8 SER CA C 54.3 0.2 1 46 108 8 SER CB C 63.2 0.2 1 47 108 8 SER N N 119.0 0.2 1 48 109 9 ASP C C 172.0 0.2 1 49 109 9 ASP CA C 49.4 0.2 1 50 109 9 ASP CB C 38.8 0.2 1 51 109 9 ASP CG C 174.4 0.2 1 52 109 9 ASP N N 118.1 0.2 1 53 110 10 TYR C C 174.1 0.2 1 54 110 10 TYR CA C 54.5 0.2 1 55 110 10 TYR CB C 41.0 0.2 1 56 110 10 TYR CG C 129.5 0.2 1 57 110 10 TYR CD1 C 130.8 0.2 3 58 110 10 TYR CD2 C 130.8 0.2 3 59 110 10 TYR CE1 C 116.1 0.2 3 60 110 10 TYR CE2 C 116.1 0.2 3 61 110 10 TYR CZ C 154.8 0.2 1 62 110 10 TYR N N 130.6 0.2 1 63 111 11 SER C C 169.8 0.2 1 64 111 11 SER CA C 55.9 0.2 1 65 111 11 SER CB C 67.1 0.2 1 66 111 11 SER N N 121.8 0.2 1 67 112 12 LYS C C 172.7 0.2 1 68 112 12 LYS CA C 53.6 0.2 1 69 112 12 LYS CB C 34.6 0.2 1 70 112 12 LYS CG C 23.4 0.2 1 71 112 12 LYS CD C 27.8 0.2 1 72 112 12 LYS CE C 40.4 0.2 1 73 112 12 LYS N N 124.0 0.2 1 74 112 12 LYS NZ N 33.7 0.2 1 75 113 13 TYR C C 173.1 0.2 1 76 113 13 TYR CA C 54.7 0.2 1 77 113 13 TYR CB C 38.7 0.2 1 78 113 13 TYR CG C 128.4 0.2 1 79 113 13 TYR CD1 C 130.9 0.2 3 80 113 13 TYR CD2 C 130.9 0.2 3 81 113 13 TYR CE1 C 116.0 0.2 3 82 113 13 TYR CE2 C 116.0 0.2 3 83 113 13 TYR CZ C 155.5 0.2 1 84 113 13 TYR N N 120.8 0.2 1 85 114 14 LEU C C 173.6 0.2 1 86 114 14 LEU CA C 53.0 0.2 1 87 114 14 LEU CB C 43.4 0.2 1 88 114 14 LEU CG C 25.9 0.2 1 89 114 14 LEU CD1 C 23.6 0.2 2 90 114 14 LEU CD2 C 23.4 0.2 2 91 114 14 LEU N N 126.7 0.2 1 92 115 15 ASP C C 171.9 0.2 1 93 115 15 ASP CA C 51.3 0.2 1 94 115 15 ASP CB C 41.1 0.2 1 95 115 15 ASP CG C 175.4 0.2 1 96 115 15 ASP N N 123.4 0.2 1 97 116 16 SER C C 171.9 0.2 1 98 116 16 SER CA C 55.4 0.2 1 99 116 16 SER CB C 64.4 0.2 1 100 116 16 SER N N 120.3 0.2 1 101 117 17 ARG C C 173.4 0.2 1 102 117 17 ARG CA C 53.3 0.2 1 103 117 17 ARG CB C 32.5 0.2 1 104 117 17 ARG CG C 25.6 0.2 1 105 117 17 ARG CD C 42.1 0.2 1 106 117 17 ARG CZ C 158.3 0.2 1 107 117 17 ARG N N 123.6 0.2 1 108 117 17 ARG NE N 85.6 0.2 1 109 117 17 ARG NH1 N 72.5 0.2 2 110 117 17 ARG NH2 N 72.5 0.2 2 111 118 18 ARG C C 172.0 0.2 1 112 118 18 ARG CA C 53.2 0.2 1 113 118 18 ARG CB C 32.9 0.2 1 114 118 18 ARG CG C 26.2 0.2 1 115 118 18 ARG CD C 42.0 0.2 1 116 118 18 ARG CZ C 158.3 0.2 1 117 118 18 ARG N N 127.5 0.2 1 118 118 18 ARG NE N 85.6 0.2 1 119 118 18 ARG NH1 N 72.5 0.2 2 120 118 18 ARG NH2 N 72.5 0.2 2 121 119 19 ALA C C 174.1 0.2 1 122 119 19 ALA CA C 49.5 0.2 1 123 119 19 ALA CB C 21.2 0.2 1 124 119 19 ALA N N 126.2 0.2 1 125 120 20 GLN C C 171.4 0.2 1 126 120 20 GLN CA C 52.9 0.2 1 127 120 20 GLN CB C 31.0 0.2 1 128 120 20 GLN CG C 32.0 0.2 1 129 120 20 GLN CD C 178.9 0.2 1 130 120 20 GLN N N 119.9 0.2 1 131 120 20 GLN NE2 N 112.4 0.2 1 132 121 21 ASP C C 171.6 0.2 1 133 121 21 ASP CA C 50.5 0.2 1 134 121 21 ASP CB C 40.0 0.2 1 135 121 21 ASP CG C 174.2 0.2 1 136 121 21 ASP N N 125.9 0.2 1 137 122 22 PHE C C 171.7 0.2 1 138 122 22 PHE CA C 54.1 0.2 1 139 122 22 PHE CB C 41.2 0.2 1 140 122 22 PHE CG C 136.5 0.2 1 141 122 22 PHE CD1 C 130.4 0.2 3 142 122 22 PHE CD2 C 130.4 0.2 3 143 122 22 PHE CE1 C 129.8 0.2 3 144 122 22 PHE CE2 C 129.8 0.2 3 145 122 22 PHE CZ C 128.8 0.2 1 146 122 22 PHE N N 127.9 0.2 1 147 123 23 VAL C C 171.9 0.2 1 148 123 23 VAL CA C 59.4 0.2 1 149 123 23 VAL CB C 34.7 0.2 1 150 123 23 VAL CG1 C 20.4 0.2 2 151 123 23 VAL CG2 C 19.0 0.2 2 152 123 23 VAL N N 124.0 0.2 1 153 124 24 GLN C C 172.2 0.2 1 154 124 24 GLN CA C 52.4 0.2 1 155 124 24 GLN CB C 32.5 0.2 1 156 124 24 GLN CG C 32.5 0.2 1 157 124 24 GLN CD C 179.5 0.2 1 158 124 24 GLN N N 125.1 0.2 1 159 124 24 GLN NE2 N 112.4 0.2 1 160 125 25 TRP C C 172.2 0.2 1 161 125 25 TRP CA C 54.3 0.2 1 162 125 25 TRP CB C 29.2 0.2 1 163 125 25 TRP CG C 109.2 0.2 1 164 125 25 TRP CD1 C 122.8 0.2 1 165 125 25 TRP CD2 C 130.6 0.2 1 166 125 25 TRP CE2 C 136.0 0.2 1 167 125 25 TRP CE3 C 117.7 0.2 1 168 125 25 TRP CZ2 C 111.0 0.2 1 169 125 25 TRP CZ3 C 119.4 0.2 1 170 125 25 TRP CH2 C 121.7 0.2 1 171 125 25 TRP N N 122.5 0.2 1 172 125 25 TRP NE1 N 131.0 0.2 1 173 126 26 LEU C C 173.4 0.2 1 174 126 26 LEU CA C 53.4 0.2 1 175 126 26 LEU CB C 43.6 0.2 1 176 126 26 LEU CG C 26.1 0.2 1 177 126 26 LEU CD1 C 23.8 0.2 2 178 126 26 LEU CD2 C 21.3 0.2 2 179 126 26 LEU N N 122.3 0.2 1 180 127 27 MET C C 172.6 0.2 1 181 127 27 MET CA C 52.7 0.2 1 182 127 27 MET CB C 36.0 0.2 1 183 127 27 MET CG C 30.9 0.2 1 184 127 27 MET CE C 14.8 0.2 1 185 127 27 MET N N 121.2 0.2 1 186 128 28 ASN C C 172.7 0.2 1 187 128 28 ASN CA C 51.5 0.2 1 188 128 28 ASN CB C 41.3 0.2 1 189 128 28 ASN CG C 174.7 0.2 1 190 128 28 ASN N N 116.6 0.2 1 191 128 28 ASN ND2 N 119.8 0.2 1 192 129 29 THR C C 178.2 0.2 1 193 129 29 THR CA C 60.2 0.2 1 194 129 29 THR CB C 69.6 0.2 1 195 129 29 THR CG2 C 20.0 0.2 1 196 129 29 THR N N 119.6 0.2 1 stop_ save_