data_26679 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone resonance assignments of pyroglutamate Abeta(3-42) in 50 % trifluoroethanol ; _BMRB_accession_number 26679 _BMRB_flat_file_name bmr26679.str _Entry_type original _Submission_date 2015-10-06 _Accession_date 2015-10-06 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Dammers Christina . . 2 Willbold Dieter . . 3 Reiss Kerstin . . 4 Lecher Justin . . 5 Stoldt Matthias . . 6 Schwarten Melanie . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 40 "13C chemical shifts" 79 "15N chemical shifts" 40 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-12-17 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 26678 Amyloid-beta(1-42) 26680 pEAbeta(3-42) stop_ _Original_release_date 2015-12-17 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Structural Analysis and Aggregation Propensity of Pyroglutamate Abeta(3-40) in Aqueous Trifluoroethanol ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26600248 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Dammers Christina . . 2 Reiss Kerstin . . 3 Gremer Lothar . . 4 Lecher Justin . . 5 Ziehm Tamar . . 6 Stoldt Matthias . . 7 Schwarten Melanie . . 8 Willbold Dieter . . stop_ _Journal_abbreviation 'PLoS One' _Journal_volume 10 _Journal_issue 11 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first e0143647 _Page_last e0143647 _Year 2015 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name pEAbeta(3-42) _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label pEAb42 $pEAb42 stop_ _System_molecular_weight 4310.9081 _System_physical_state unfolded _System_oligomer_state ? _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_pEAb42 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common pEAb42 _Molecular_mass 4310.9081 _Mol_thiol_state 'not present' _Details 'molecule starts with pyroglutamate (X) at position 3' ############################## # Polymer residue sequence # ############################## _Residue_count 40 _Mol_residue_sequence ; XFRHDSGYEVHHQKLVFFAE DVGSNKGAIIGLMVGGVVIA ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 3 PCA 2 4 PHE 3 5 ARG 4 6 HIS 5 7 ASP 6 8 SER 7 9 GLY 8 10 TYR 9 11 GLU 10 12 VAL 11 13 HIS 12 14 HIS 13 15 GLN 14 16 LYS 15 17 LEU 16 18 VAL 17 19 PHE 18 20 PHE 19 21 ALA 20 22 GLU 21 23 ASP 22 24 VAL 23 25 GLY 24 26 SER 25 27 ASN 26 28 LYS 27 29 GLY 28 30 ALA 29 31 ILE 30 32 ILE 31 33 GLY 32 34 LEU 33 35 MET 34 36 VAL 35 37 GLY 36 38 GLY 37 39 VAL 38 40 VAL 39 41 ILE 40 42 ALA stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_PCA _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'PYROGLUTAMIC ACID' _BMRB_code PCA _PDB_code PCA _Standard_residue_derivative . _Molecular_mass 129.114 _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 . ? CD CD C . 0 . ? OE OE O . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 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 CD ? ? SING N H ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? DOUB CD OE ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $pEAb42 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 _Variant _Vector_name $pEAb42 'recombinant technology' 'Escherichia coli' Escherichia coli human pLysS pRSET stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '50 % trifluorethanol, pH 2.8' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $pEAb42 0.1 mM '[U-13C; U-15N]' TFE 50 % [U-2H] 'potassium phosphate' 50 mM 'natural abundance' H2O 50 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr_Analysis _Saveframe_category software _Name CcpNmr_Analysis _Version 2.4 loop_ _Vendor _Address _Electronic_address CCPN 'Department of Biochemistry, Cambridge CB2 1GA, UK' http://www.ccpn.ac.uk stop_ loop_ _Task 'chemical shift assignment' stop_ _Details 'The CCPN NMR assignment and data analysis application' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_3D_HNCO_1 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC/HMQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC/HMQC' _Sample_label $sample_1 save_ save_3D_HNCA_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_aqueous_trifluoroethanol _Saveframe_category sample_conditions _Details '50 % trifluoroethanol, 50 mM potassium phosphate' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.050 . M pH 2.800 . pH pressure 1.000 . atm temperature 293.150 . 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 carbons' ppm 0.0 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '3D HNCO' '2D 1H-15N HSQC/HMQC' '3D HNCA' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $aqueous_trifluoroethanol _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name pEAb42 _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 3 1 PCA H H 7.780 0.002 1 2 3 1 PCA C C 176.437 0.02 1 3 3 1 PCA CA C 59.592 0.001 1 4 3 1 PCA N N 123.506 0.017 1 5 4 2 PHE H H 7.926 0.002 1 6 4 2 PHE C C 174.850 0.02 1 7 4 2 PHE CA C 57.381 0.033 1 8 4 2 PHE N N 118.197 0.025 1 9 5 3 ARG H H 8.293 0.001 1 10 5 3 ARG C C 175.285 0.02 1 11 5 3 ARG CA C 56.320 0.002 1 12 5 3 ARG N N 121.061 0.014 1 13 6 4 HIS H H 8.592 0.003 1 14 6 4 HIS C C 173.162 0.02 1 15 6 4 HIS CA C 55.467 0.017 1 16 6 4 HIS N N 118.964 0.021 1 17 7 5 ASP H H 8.476 0.002 1 18 7 5 ASP C C 175.135 0.02 1 19 7 5 ASP CA C 53.425 0.0 1 20 7 5 ASP N N 120.149 0.023 1 21 8 6 SER H H 8.497 0.003 1 22 8 6 SER C C 174.676 0.02 1 23 8 6 SER CA C 59.913 0.003 1 24 8 6 SER N N 117.025 0.023 1 25 9 7 GLY H H 8.617 0.002 1 26 9 7 GLY C C 174.964 0.02 1 27 9 7 GLY CA C 46.620 0.019 1 28 9 7 GLY N N 109.690 0.023 1 29 10 8 TYR H H 8.109 0.003 1 30 10 8 TYR C C 177.198 0.02 1 31 10 8 TYR CA C 61.022 0.007 1 32 10 8 TYR N N 121.679 0.025 1 33 11 9 GLU H H 8.387 0.015 1 34 11 9 GLU C C 177.481 0.02 1 35 11 9 GLU CA C 58.919 0.019 1 36 11 9 GLU N N 119.963 0.074 1 37 12 10 VAL H H 8.203 0.005 1 38 12 10 VAL C C 176.890 0.02 1 39 12 10 VAL CA C 65.546 0.135 1 40 12 10 VAL N N 119.464 0.014 1 41 13 11 HIS H H 8.114 0.003 1 42 13 11 HIS C C 175.166 0.02 1 43 13 11 HIS CA C 58.557 0.002 1 44 13 11 HIS N N 117.077 0.027 1 45 14 12 HIS H H 8.521 0.004 1 46 14 12 HIS C C 174.619 0.02 1 47 14 12 HIS CA C 58.759 0.005 1 48 14 12 HIS N N 117.009 0.147 1 49 15 13 GLN H H 8.351 0.002 1 50 15 13 GLN C C 176.708 0.02 1 51 15 13 GLN CA C 58.555 0.031 1 52 15 13 GLN N N 118.695 0.04 1 53 16 14 LYS H H 8.093 0.002 1 54 16 14 LYS C C 177.215 0.02 1 55 16 14 LYS CA C 59.291 0.059 1 56 16 14 LYS N N 118.643 0.039 1 57 17 15 LEU H H 7.709 0.002 1 58 17 15 LEU C C 177.693 0.02 1 59 17 15 LEU CA C 57.813 0.014 1 60 17 15 LEU N N 119.645 0.026 1 61 18 16 VAL H H 7.834 0.003 1 62 18 16 VAL C C 176.891 0.02 1 63 18 16 VAL CA C 66.158 0.043 1 64 18 16 VAL N N 119.061 0.02 1 65 19 17 PHE H H 8.103 0.003 1 66 19 17 PHE C C 176.927 0.02 1 67 19 17 PHE CA C 60.173 0.144 1 68 19 17 PHE N N 119.121 0.151 1 69 20 18 PHE H H 8.401 0.012 1 70 20 18 PHE C C 176.368 0.02 1 71 20 18 PHE CA C 60.948 0.137 1 72 20 18 PHE N N 120.026 0.032 1 73 21 19 ALA H H 8.677 0.002 1 74 21 19 ALA C C 179.584 0.02 1 75 21 19 ALA CA C 55.054 0.035 1 76 21 19 ALA N N 121.898 0.027 1 77 22 20 GLU H H 8.415 0.002 1 78 22 20 GLU C C 176.985 0.02 1 79 22 20 GLU CA C 57.763 0.032 1 80 22 20 GLU N N 115.831 0.022 1 81 23 21 ASP H H 8.272 0.003 1 82 23 21 ASP C C 176.062 0.02 1 83 23 21 ASP CA C 55.004 0.012 1 84 23 21 ASP N N 118.973 0.02 1 85 24 22 VAL H H 8.185 0.002 1 86 24 22 VAL C C 177.093 0.02 1 87 24 22 VAL CA C 65.009 0.0 1 88 24 22 VAL N N 119.501 0.058 1 89 25 23 GLY H H 8.215 0.002 1 90 25 23 GLY C C 174.411 0.02 1 91 25 23 GLY CA C 46.241 0.01 1 92 25 23 GLY N N 107.331 0.032 1 93 26 24 SER H H 7.930 0.002 1 94 26 24 SER C C 174.066 0.02 1 95 26 24 SER CA C 59.369 0.011 1 96 26 24 SER N N 114.734 0.018 1 97 27 25 ASN H H 8.096 0.003 1 98 27 25 ASN C C 174.540 0.02 1 99 27 25 ASN CA C 53.845 0.017 1 100 27 25 ASN N N 120.129 0.024 1 101 28 26 LYS H H 8.271 0.003 1 102 28 26 LYS C C 176.647 0.02 1 103 28 26 LYS CA C 58.601 0.007 1 104 28 26 LYS N N 120.940 0.043 1 105 29 27 GLY H H 8.378 0.001 1 106 29 27 GLY C C 174.611 0.02 1 107 29 27 GLY CA C 46.469 0.001 1 108 29 27 GLY N N 105.693 0.024 1 109 30 28 ALA H H 7.824 0.002 1 110 30 28 ALA C C 178.219 0.02 1 111 30 28 ALA CA C 54.233 0.016 1 112 30 28 ALA N N 123.225 0.022 1 113 31 29 ILE H H 7.715 0.002 1 114 31 29 ILE C C 176.612 0.02 1 115 31 29 ILE CA C 63.540 0.024 1 116 31 29 ILE N N 117.303 0.02 1 117 32 30 ILE H H 7.975 0.002 1 118 32 30 ILE C C 177.160 0.02 1 119 32 30 ILE CA C 64.141 0.066 1 120 32 30 ILE N N 120.457 0.019 1 121 33 31 GLY H H 8.036 0.002 1 122 33 31 GLY C C 175.247 0.02 1 123 33 31 GLY CA C 46.890 0.003 1 124 33 31 GLY N N 106.183 0.03 1 125 34 32 LEU H H 7.913 0.002 1 126 34 32 LEU C C 178.186 0.02 1 127 34 32 LEU CA C 57.206 0.002 1 128 34 32 LEU N N 121.432 0.025 1 129 35 33 MET H H 8.230 0.002 1 130 35 33 MET C C 177.830 0.02 1 131 35 33 MET CA C 57.936 0.003 1 132 35 33 MET N N 118.915 0.037 1 133 36 34 VAL H H 8.508 0.002 1 134 36 34 VAL C C 176.845 0.02 1 135 36 34 VAL CA C 64.203 0.028 1 136 36 34 VAL N N 117.816 0.019 1 137 37 35 GLY H H 8.092 0.002 1 138 37 35 GLY C C 174.036 0.02 1 139 37 35 GLY CA C 45.863 0.016 1 140 37 35 GLY N N 107.679 0.023 1 141 38 36 GLY H H 7.999 0.002 1 142 38 36 GLY C C 173.212 0.02 1 143 38 36 GLY CA C 45.629 0.007 1 144 38 36 GLY N N 107.247 0.03 1 145 39 37 VAL H H 7.828 0.002 1 146 39 37 VAL C C 174.965 0.02 1 147 39 37 VAL CA C 62.867 0.006 1 148 39 37 VAL N N 118.808 0.025 1 149 40 38 VAL H H 7.829 0.003 1 150 40 38 VAL C C 174.736 0.02 1 151 40 38 VAL CA C 62.472 0.003 1 152 40 38 VAL N N 121.692 0.023 1 153 41 39 ILE H H 7.897 0.002 1 154 41 39 ILE C C 174.341 0.02 1 155 41 39 ILE CA C 60.853 0.054 1 156 41 39 ILE N N 122.674 0.03 1 157 42 40 ALA H H 7.911 0.002 1 158 42 40 ALA CA C 51.500 0.02 1 159 42 40 ALA N N 127.082 0.026 1 stop_ save_